C- and Z-Shaped Coordination Compounds. Synthesis, Structure, and Spectroelectrochemistry of cis- and trans-[Re(CO)3(L)]2-2,2'-bisbenzimidizolate with L = 4-Phenylpyridine, 2,4'-Bipyridine, or Pyridine
Peter H. Dinolfo; Kurt D. Benkstein; Charlotte L. Stern; Joseph T. Hupp; Inorganic Chemistry 44 (2005) 8707–8714; doi:10.1021/ic050894u

data_4310062
_publ_section_title
;
C- and Z-Shaped Coordination Compounds. Synthesis, Structure, and
Spectroelectrochemistry of cis-
and trans-[Re(CO)3(L)]2-2,2'-bisbenzimidizolate with L = 4-Phenylpyridine,
2,4'-Bipyridine, or Pyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8707
_journal_page_last               8714
_journal_paper_doi               10.1021/ic050894u
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C75 H65 N9 O10.5 Re3'
_chemical_formula_weight         1818.96
_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                 95.0500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.2442(7)
_cell_length_b                   27.6324(16)
_cell_length_c                   22.4781(12)
_cell_measurement_temperature    153(2)
_cell_volume                     7575.6(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_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  0.0769
_diffrn_reflns_av_sigmaI/netI    0.0934
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            69472
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.17
_exptl_absorpt_coefficient_mu    4.843
_exptl_absorpt_correction_T_max  0.8241
_exptl_absorpt_correction_T_min  0.6485
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3548
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.50
_refine_diff_density_max         1.946
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         18173
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.173
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                11054
_reflns_number_total             18173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050894usi20050602_034818_1.cif
_cod_data_source_block           1trans
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

Disordered hexane molecule was marked as such according to the text of
the original publication. Tag _atom_site_attached_hydrogens was added
with numbers of attached hydrogens for the hexane molecules. As a result,
published and calculated summary formulae match.

Andrius Merkys
2015-09-15
;
_cod_original_formula_sum        'C75 H65 N9 O10.50 Re3'
_cod_database_code               4310062