Unprecedented Polycrystal Structure of a New Cadmium Thiolate Containing an Unusually Highly Charged [ClCd8{SCH(CH2CH2)2N(H)Me}16]15+ Core
Pilar Gonzàlez-Duarte; William Clegg; Isidre Casals; Joan Sola; Jordi Rius; Journal of the American Chemical Society 120 (1998) 1260–1266; doi:10.1021/ja972038q

data_4116684
_publ_section_title
;
 Unprecedented Polycrystal Structure of a New Cadmium Thiolate Containing
 an Unusually Highly Charged [ClCd8{SCH(CH2CH2)2N(H)Me}16]15+ Core
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1260
_journal_page_last               1266
_journal_paper_doi               10.1021/ja972038q
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C96 H240 Cd8 Cl16 N16 O76 S16'
_chemical_formula_weight         4814.40
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.707(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.319(2)
_cell_length_b                   24.0998(14)
_cell_length_c                   26.2568(15)
_cell_measurement_reflns_used    21821
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.10
_cell_volume                     19164(2)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48933
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.08
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  0.557
_exptl_absorpt_correction_T_min  0.426
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       block
_exptl_crystal_F_000             9792
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.199
_refine_ls_extinction_coef       0.00014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         16325
_refine_ls_number_restraints     1636
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.1238
_refine_ls_R_factor_obs          0.0901
_refine_ls_shift/esd_max         0.935
_refine_ls_shift/esd_mean        0.015
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1524P)^2^+245.6854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3047
_refine_ls_wR_factor_obs         0.2492
_reflns_number_observed          11851
_reflns_number_total             16798
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja972038q.cif
_cod_data_source_block           pg29a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1524P)^2^+245.6854P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1524P)^2^+245.6854P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        19163.8(19)
_cod_database_code               4116684