Dianiline-1κ<i>N</i>,2κ<i>N</i>-bis[3,4(η^5^)-pentamethylcyclopentadienyl]tetra-μ~3~-sulfido-<i>tetrahedro</i>-dicopper(I)dimolybdenum(V) bis(perchlorate) aniline hemisolvate
Ren, Zhi-Gang; Lang, Jian-Ping; Ng, Seik Weng; Acta Crystallographica Section E 63 (2007) m1020–m1022; doi:10.1107/S1600536807010847

data_2212878
_publ_section_title
;Dianiline-1\k<i>N</i>,2\k<i>N</i>-bis[3,4(\h^5^)-pentamethylcyclopentadienyl]tetra-\m~3~-sulfido-<i>tetrahedro</i>-dicopper(I)dimolybdenum(V)
 bis(perchlorate) aniline hemisolvate
;
_journal_coeditor_code           GK2061
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1020
_journal_page_last               m1022
_journal_paper_doi               10.1107/S1600536807010847
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety
'C32 H44 Cu2 Mo2 N2 S4 2+ , 2Cl O4 - , 0.5C6 H7 N'
_chemical_formula_sum            'C35 H47.5 Cl2 Cu2 Mo2 N2.5 O8 S4'
_chemical_formula_weight         1149.35
_chemical_name_systematic
;
Dianiline-1\kN,2\kN-bis[3,4-(\h^5^)-pentamethylcyclopentadienyl]tetra-\m~3~-
sulfido-tetrahedro-dicopper(I)dimolybdenum(V) bis(perchlorate) aniline
hemisolvate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.680(2)
_cell_length_b                   18.303(4)
_cell_length_c                   20.716(4)
_cell_measurement_reflns_used    14605
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.2
_cell_volume                     4322.8(15)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_diffrn_measurement_device_type  'Rigaku Mercury CCD area-detector'
_diffrn_measurement_method       \w
_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  0.041
_diffrn_reflns_av_sigmaI/netI    0.032
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41698
_diffrn_reflns_theta_full        25.4
_diffrn_reflns_theta_max         25.4
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.905
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7879
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.11
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0364P)^2^+6.7353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.082
_refine_ls_wR_factor_ref         0.086
_reflns_number_gt                7172
_reflns_number_total             7879
_reflns_threshold_expression     I>\2(I)
_cod_data_source_file            gk2061.cif
_cod_data_source_block           I
_cod_original_cell_volume        4322.9(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C35 H47.50 Cl2 Cu2 Mo2 N2.50 O8 S4'
_cod_database_code               2212878
_cod_database_fobs_code          2212878