data_Pb2W_4

# publcif _publ_body_element loop start
loop_
_publ_body_element
_publ_body_title
_publ_body_contents

 section 
;
Introduction
; 
;

;
 section 
;
Experimental
; 
;

;
 subsection 
;
Synthesis and crystallization
; 
;

;
 subsection 
;
Refinement
;
;
Crystal data, data collection and structure refinement details are summarized
in Table 1.
;

 section 
;
Results and discussion
; 
;

;
# publcif _publ_body_element loop end

_publ_section_related_literature ?

_publ_contact_author_name 'Dan Holtstam'

_publ_contact_letter 
;
Please consider this CIF for publication. I certify that this contibution is the
original work of those listed as authors; that it has not been published
before (in any language or medium) and is not being considered for publication
elsewhere; that all authors concur with and are aware of the submission; that
all workers involved in the study are listed as authors or given proper credit
in the acknowledgements; that I have obtained permission for and acknowledged
the source of any excerpts from other copyright works; and that to the best of
my knowledge the paper contains no statements which are libellous, unlawful or
in any way actionable. All coauthors have made significant scientific
contributions to the work reported, including the ideas and their execution,
and share responsibility and accountability for the results.
;


_publ_requested_category ?

_publ_requested_journal ?

_publ_contact_author_fax ?

_publ_contact_author_phone ?

_publ_contact_author_address

;
Department of Geosciences, Swedish Museum of Natural History, Box 50007, SE-104 05 Stockholm, Sweden
;


_publ_section_title
;
anghofite, Pb4[W2O8(OH)2](OH)2, a new mineral from Långban, Sweden
;

# Loop of author details

loop_
_publ_author_name
_publ_author_address
_publ_author_footnote
_publ_author_email
'Holtstam, Dan'
;
Department of Geosciences, Swedish Museum of Natural History, Box 50007, SE-104
05 Stockholm, Sweden
;
.
;
dan.holtstam@nrm.se
;
'Camara, Fernando'
;
Dipartimento di Scienze della Terra "A. Desio"
Università degli Studi di Milano Via Mangiagalli, 34 - 20133 Milano, Italy
;
.
;
fernando.camara@unimi.it
;
'Karlsson, Andreas'
;
Department of Geosciences, Swedish Museum of Natural History, Box 50007, SE-104
05 Stockholm, Sweden
;
.
.






_publ_contact_author_email
'dan.holtstam@nrm.se'
#Added by publCIF



_audit_update_record
;
2020-01-21 # Formatted by publCIF

;


 
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'H2 O6 Pb2 W' 
_chemical_formula_sum
 'H2 O6 Pb2 W' 
_chemical_formula_weight          697.25

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Pb'  'Pb'  -3.3944  10.1111
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    6.61540(10)
_cell_length_b                    7.07660(10)
_cell_length_c                    7.32960(10)
_cell_angle_alpha                 118.175(2)
_cell_angle_beta                  94.4510(10)
_cell_angle_gamma                 101.1460(10)
_cell_volume                      291.056(9)
_cell_formula_units_Z             2
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used   19112
_cell_measurement_theta_min     3.1970
_cell_measurement_theta_max     40.2340
 
_exptl_crystal_description        lath
_exptl_crystal_colour             colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     7.956          
_exptl_crystal_F_000              578
_exptl_crystal_size_max           0.146
_exptl_crystal_size_mid           0.090
_exptl_crystal_size_min           0.010
_exptl_absorpt_coefficient_mu     77.371
_shelx_estimated_absorpt_T_min    0.031
_shelx_estimated_absorpt_T_max    0.512
_exptl_absorpt_correction_T_min   0.02795
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.62a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min           0.425
_oxdiff_exptl_absorpt_empirical_full_max          14.191
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'micro-focus sealed X-ray tube'
_diffrn_source_type               'PhotonJet (Mo) X-ray Source'
_diffrn_radiation_probe           x-ray
_diffrn_radiation_monochromator   mirror
_diffrn_measurement_device        'four-circle diffractometer'
_diffrn_measurement_device_type   'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_detector                  'Hybrid Pixel Array Detector'
_diffrn_detector_type             HyPix
_diffrn_detector_area_resol_mean  10.0000
_diffrn_reflns_number             29035
_diffrn_reflns_av_unetI/netI      0.0198
_diffrn_reflns_av_R_equivalents   0.0400
_diffrn_reflns_limit_h_min        -12
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13
_diffrn_reflns_theta_min          3.200
_diffrn_reflns_theta_max          40.438
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.982
_diffrn_measured_fraction_theta_full  0.994
_diffrn_reflns_Laue_measured_fraction_max    0.982
_diffrn_reflns_Laue_measured_fraction_full   0.994
_diffrn_reflns_point_group_measured_fraction_max   0.982
_diffrn_reflns_point_group_measured_fraction_full  0.994
_diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0083080000
_diffrn_orient_matrix_UB_12       0.0734575000
_diffrn_orient_matrix_UB_13       0.1047080000
_diffrn_orient_matrix_UB_21       0.0118170000
_diffrn_orient_matrix_UB_22       0.0879950000
_diffrn_orient_matrix_UB_23      -0.0227756000
_diffrn_orient_matrix_UB_31      -0.1104858000
_diffrn_orient_matrix_UB_32      -0.0271997000
_diffrn_orient_matrix_UB_33      -0.0323521000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -41.00  82.00   0.50    2.40    --   -0.39  57.00   0.00  246
  2  ω     71.00 129.00   0.50    8.40    --   47.87 125.00  60.00  116
  3  ω     71.00 129.00   0.50    8.40    --   47.87 125.00 120.00  116
  4  ω      1.00 129.00   0.50    8.40    --   47.87  77.00  60.00  256
  5  ω      1.00 129.00   0.50    8.40    --   47.87  77.00 120.00  256
  6  ω      1.00 129.00   0.50    8.40    --   47.87  77.00 -30.00  256
  7  ω      1.00 129.00   0.50    8.40    --   47.87  77.00-120.00  256
  8  ω      1.00 129.00   0.50    8.40    --   47.87  77.00 -60.00  256
  9  ω      1.00 117.00   0.50    8.40    --   47.87  77.00 150.00  232
 10  ω     10.00 117.00   0.50    8.40    --   47.87-125.00-120.00  214
 11  ω     36.00  82.00   0.50    2.40    --   -0.39-178.00 -30.00   92
 12  ω     36.00  82.00   0.50    2.40    --   -0.39-178.00 -90.00   92
 13  ω     10.00 117.00   0.50    8.40    --   47.87-125.00   0.00  214
 14  ω     10.00 117.00   0.50    8.40    --   47.87-125.00  90.00  214
 15  ω    -26.00 106.00   0.50    8.40    --   47.87 -99.00-150.00  264
 16  ω    -26.00 106.00   0.50    8.40    --   47.87 -99.00 -90.00  264
 17  ω    -35.00  44.00   0.50    8.40    --   47.87 -57.00   0.00  158
 18  ω    -50.00   3.00   0.50    8.40    --   47.87 -10.00  38.00  106
 19  ω    -46.00  84.00   0.50    8.40    --   47.87 -77.00  60.00  260
 20  ω    -46.00 129.00   0.50    8.40    --   47.87  10.00-147.00  350
 21  ω    -46.00  34.00   0.50    8.40    --  -48.65  10.00-147.00  160
 22  ω    -46.00  82.00   0.50    2.40    --   -0.39  10.00-147.00  256
 23  ω    -47.00   5.00   0.50    8.40    --   47.87 -19.00 -30.00  104
 24  ω    -98.00   3.00   0.50    2.40    --   -0.39 -10.00  38.00  202
 25  ω    -64.00  34.00   0.50    8.40    --  -48.65  37.00 120.00  196
 26  ω    -95.00  34.00   0.50    8.40    --  -48.65  77.00-120.00  258
 27  ω    -95.00  34.00   0.50    8.40    --  -48.65  77.00  90.00  258
 28  ω   -132.00  -9.00   0.50    8.40    --  -48.65 -57.00 150.00  246
 29  ω   -101.00 -38.00   0.50    2.40    --   -0.39-178.00  90.00  126
 30  ω   -142.00 -83.00   0.50    8.40    --  -48.65 -99.00  30.00  118
 31  ω   -135.00 -70.00   0.50    8.40    --  -48.65-125.00  90.00  130
 32  ω   -146.00   3.00   0.50    8.40    --  -48.65 -10.00  38.00  298
;
_diffrn_measurement_method 'ω scans'
_diffrn_oxdiff_digest_frames
;
0137efc8ddace56dec49a09ca742be898f000278f55
;
_diffrn_oxdiff_digest_hkl
;
01b42fb6cf05ea0135c3f25f0178496afececf
;
_reflns_number_total              3647
_reflns_number_gt                 3360
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_audit_creation_date           2019-12-11
_audit_creation_method         'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_collection     'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_cell_refinement     'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_data_reduction      'CrysAlisPro 1.171.40.16b (Rigaku OD, 2018)'
_computing_structure_solution    'superflip (Palatinus and Cahpuis, 2007)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0187P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef        0.00294(14)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_number_reflns          3647
_refine_ls_number_parameters      86
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0190
_refine_ls_R_factor_gt            0.0163
_refine_ls_wR_factor_ref          0.0374
_refine_ls_wR_factor_gt           0.0366
_refine_ls_goodness_of_fit_ref    1.034
_refine_ls_restrained_S_all       1.034
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Pb1 Pb 0.35798(2) 0.22210(2) 0.48875(2) 0.01868(3) Uani 1 1 d . . . . .
Pb2 Pb 0.26698(2) 0.29219(2) 1.00803(2) 0.01748(3) Uani 0.9983(8) 1 d . . P . .
W1 W 0.82374(2) 0.31638(2) 0.28718(2) 0.01304(3) Uani 0.9964(9) 1 d . . P . .
O1 O 0.1940(3) 0.8502(4) 0.9873(3) 0.0197(4) Uani 1 1 d . . . . .
O2 O 0.8806(3) 0.5872(4) 0.6248(3) 0.0161(3) Uani 1 1 d . . . . .
O3 O 0.7674(3) 0.1137(4) 0.3672(3) 0.0203(4) Uani 1 1 d . . . . .
O4 O 0.5601(3) 0.3865(4) 0.3013(3) 0.0158(3) Uani 1 1 d . . . . .
OH1 O 0.1187(3) 0.3768(4) 0.7379(3) 0.0181(3) Uani 1 1 d . . . . .
OH2 O 0.5635(3) 0.3291(4) 0.8275(3) 0.0181(3) Uani 1 1 d . . . . .
H2 H 0.684100 0.298500 0.846900 0.022 Uiso 1 1 d . U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
Pb1 O4 2.366(2) 2_666 ?
Pb1 OH2 2.427(2) . ?
Pb1 O4 2.495(2) . ?
Pb1 OH1 2.504(2) . ?
Pb1 O2 2.5853(19) 2_666 ?
Pb1 W1 3.40126(16) 2_666 ?
Pb2 OH2 2.339(2) 2_667 ?
Pb2 OH2 2.490(2) . ?
Pb2 OH1 2.507(2) . ?
Pb2 O4 2.5144(18) 1_556 ?
Pb2 O2 2.7358(19) 2_667 ?
W1 O1 1.767(2) 2_666 ?
W1 O3 1.778(2) . ?
W1 O2 1.8922(18) 2_766 ?
W1 O4 1.9009(18) . ?
W1 OH1 2.227(2) 2_666 ?
W1 O2 2.244(2) . ?
 
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_atom_site_label_2
 _geom_angle_atom_site_label_3
 _geom_angle
 _geom_angle_site_symmetry_1
 _geom_angle_site_symmetry_3
 _geom_angle_publ_flag
O4 Pb1 OH2 71.89(7) 2_666 . ?
O4 Pb1 O4 71.80(8) 2_666 . ?
OH2 Pb1 O4 111.31(7) . . ?
O4 Pb1 OH1 63.47(7) 2_666 . ?
OH2 Pb1 OH1 77.35(7) . . ?
O4 Pb1 OH1 128.99(7) . . ?
O4 Pb1 O2 64.48(6) 2_666 2_666 ?
OH2 Pb1 O2 132.10(7) . 2_666 ?
O4 Pb1 O2 73.23(6) . 2_666 ?
OH1 Pb1 O2 66.41(6) . 2_666 ?
O4 Pb1 W1 32.64(4) 2_666 2_666 ?
OH2 Pb1 W1 90.86(5) . 2_666 ?
O4 Pb1 W1 88.10(5) . 2_666 ?
OH1 Pb1 W1 40.89(5) . 2_666 ?
O2 Pb1 W1 41.28(4) 2_666 2_666 ?
OH2 Pb2 OH2 73.13(8) 2_667 . ?
OH2 Pb2 OH1 80.93(7) 2_667 . ?
OH2 Pb2 OH1 76.15(7) . . ?
OH2 Pb2 O4 70.76(7) 2_667 1_556 ?
OH2 Pb2 O4 82.59(6) . 1_556 ?
OH1 Pb2 O4 148.54(7) . 1_556 ?
OH2 Pb2 O2 83.51(7) 2_667 2_667 ?
OH2 Pb2 O2 148.96(6) . 2_667 ?
OH1 Pb2 O2 120.62(6) . 2_667 ?
O4 Pb2 O2 70.37(6) 1_556 2_667 ?
O1 W1 O3 101.97(11) 2_666 . ?
O1 W1 O2 99.50(9) 2_666 2_766 ?
O3 W1 O2 99.57(9) . 2_766 ?
O1 W1 O4 102.33(9) 2_666 . ?
O3 W1 O4 97.40(9) . . ?
O2 W1 O4 148.81(9) 2_766 . ?
O1 W1 OH1 91.18(9) 2_666 2_666 ?
O3 W1 OH1 166.44(9) . 2_666 ?
O2 W1 OH1 81.23(8) 2_766 2_666 ?
O4 W1 OH1 76.34(8) . 2_666 ?
O1 W1 O2 167.68(9) 2_666 . ?
O3 W1 O2 89.94(9) . . ?
O2 W1 O2 75.13(8) 2_766 . ?
O4 W1 O2 78.92(8) . . ?
OH1 W1 O2 77.13(8) 2_666 . ?
O1 W1 Pb1 124.11(7) 2_666 2_666 ?
O3 W1 Pb1 120.41(7) . 2_666 ?
O2 W1 Pb1 106.74(7) 2_766 2_666 ?
O4 W1 Pb1 42.17(6) . 2_666 ?
OH1 W1 Pb1 47.38(5) 2_666 2_666 ?
O2 W1 Pb1 49.47(5) . 2_666 ?
W1 OH1 Pb1 91.74(7) 2_666 . ?
W1 OH1 Pb2 132.65(9) 2_666 . ?
Pb1 OH1 Pb2 95.61(7) . . ?
W1 O2 W1 104.87(8) 2_766 . ?
W1 O2 Pb1 126.99(10) 2_766 2_666 ?
W1 O2 Pb1 89.25(6) . 2_666 ?
W1 O2 Pb2 104.22(8) 2_766 2_667 ?
W1 O2 Pb2 143.01(9) . 2_667 ?
Pb1 O2 Pb2 91.18(6) 2_666 2_667 ?
Pb2 OH2 Pb1 108.10(8) 2_667 . ?
Pb2 OH2 Pb2 106.87(8) 2_667 . ?
Pb1 OH2 Pb2 98.07(7) . . ?
W1 O4 Pb1 105.19(8) . 2_666 ?
W1 O4 Pb1 109.24(8) . . ?
Pb1 O4 Pb1 108.20(8) 2_666 . ?
W1 O4 Pb2 129.66(10) . 1_554 ?
Pb1 O4 Pb2 104.43(7) 2_666 1_554 ?
Pb1 O4 Pb2 98.77(6) . 1_554 ?
 
_refine_diff_density_max    1.892
_refine_diff_density_min   -1.515
_refine_diff_density_rms    0.305


loop_
_publcif_info_cif.paper_type
 ?



_publcif_funding_html
;
;
