Synthesis and structures of a triply-fused incomplete-cubane cluster [{(η5-C5Me5)WS3}3Cu7(MeCN)9](PF6)4 and a 2D polymer [(η5-C5Me5)WS3Cu3Cl(MeCN)(pz)]PF6 (pz = pyrazine)
Lang, Jian-Ping; Kawaguchi, Hiroyuki; Tatsumi, Kazuyuki; Chemical Communications  (1999) 2315–; doi:10.1039/a906081b

data_7110670
_publ_section_title
;
 Synthesis and structures of a triply-fused incomplete-cubane cluster
 [{(\h5-C5Me5)WS3}3Cu7(MeCN)9](PF6)4 and a 2D polymer
 [(\h5-C5Me5)WS3Cu3Cl(MeCN)(pz)]PF6 (pz = pyrazine)
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2315
_journal_paper_doi               10.1039/a906081b
_journal_year                    1999
_chemical_formula_sum            'C48 H72 Cu7 F24 N9 P4 S9 W3'
_chemical_formula_weight         2639.93
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_audit_creation_date             'Tue Jul 20 12:43:46 1999'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.23(1)
_cell_length_b                   31.84(1)
_cell_length_c                   20.951(8)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      6.8
_cell_measurement_theta_min      5.3
_cell_volume                     16830(11)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00259
_diffrn_orient_matrix_UB_12      0.02821
_diffrn_orient_matrix_UB_13      -0.02070
_diffrn_orient_matrix_UB_21      -0.00202
_diffrn_orient_matrix_UB_22      -0.01376
_diffrn_orient_matrix_UB_23      -0.04286
_diffrn_orient_matrix_UB_31      -0.03949
_diffrn_orient_matrix_UB_32      -0.00101
_diffrn_orient_matrix_UB_33      0.00350
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.080
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8574
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         22.48
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        -3.20
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.206
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            darkred
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             10144.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.78
_refine_diff_density_min         -0.87
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.106
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     532
_refine_ls_number_reflns         5252
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.3750
_refine_ls_shift/su_mean         0.0079
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                5252
_reflns_number_total             8572
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            906081bsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_reflns_observed_expression' tag replaced with
'_reflns_threshold_expression' tag as specified in the replacement
file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_site_calc_flags'
tag replaced with '_atom_site_calc_flag' tag as specified in the
replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

'_atom_type_scat_imag'
tag replaced with '_atom_type_scat_dispersion_imag' tag as specified
in the replacement file
'cod-tools/trunk/perl-scripts/inputs/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 3137 2015-03-23 15:08:43Z antanas 
;
_cod_original_cell_volume        16835(12)
_cod_original_sg_symbol_H-M      'P b c a      '
_cod_original_formula_sum        'C48 H72 Cu7 F24 N9 P4 S9 W3 '
_cod_database_code               7110670