X-ray Evidence of CN Bridging in Bimetallic Complexes Based on [M(CN)8]4- (M = Mo, W). The Crystal Structure of {[Mn(bpy)2]2(μ-NC)2[Mo(CN)6]2(μ-CN)2[Mn(bpy)2]2}.8H2O
Barbara Sieklucka; Janusz Szklarzewicz; Terence J. Kemp; William Errington; Inorganic Chemistry 39 (2000) 5156–5158; doi:10.1021/ic0000404

data_4321492
_publ_section_title
;
 X-ray Evidence of CN Bridging in Bimetallic Complexes Based on [M(CN)8]4-
 (M = Mo, W). The Crystal Structure of
 {[Mn(bpy)2]2(\m-NC)2[Mo(CN)6]2(\m-CN)2[Mn(bpy)2]2}.8H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5156
_journal_page_last               5158
_journal_paper_doi               10.1021/ic0000404
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C48 H40 Mn2 Mo N16 O4'
_chemical_formula_weight         1110.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.710(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9804(10)
_cell_length_b                   22.8924(12)
_cell_length_c                   15.5757(12)
_cell_measurement_reflns_used    5783
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.58
_cell_volume                     4982.7(6)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
' Siemens SMART CCD area-detector diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25498
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.9382
_exptl_absorpt_correction_T_min  0.8552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.633
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         8761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0644
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^+16.0723P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1635
_reflns_number_gt                5426
_reflns_number_total             8761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0000404.cif
_cod_data_source_block           barb2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_database_code               4321492