Paddlewheel dirhodium complexes bridged by <i>para</i>-substituted benzoates
Ebihara, Masahiro; Yamada, Kaori; Kawamura, Takashi; Acta Crystallographica Section C 62 (2006) m451–m454; doi:10.1107/S0108270106030320

data_2015550
_publ_section_title
;
 Paddlewheel dirhodium complexes bridged by <i>para</i>-substituted
 benzoates
;
_journal_coeditor_code           FG3029
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m451
_journal_page_last               m454
_journal_paper_doi               10.1107/S0108270106030320
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Rh2 (C11 H14 N O2)4 (C7 H5 N1)2] , 2C7 H5 N'
_chemical_formula_moiety         'C58 H66 N6 O8 Rh2 , 2C7 H5 N'
_chemical_formula_sum            'C72 H76 N8 O8 Rh2'
_chemical_formula_weight         1387.23
_chemical_name_systematic
;
bis(benzonitrile)tetrakis[\m-<i>p</i>-(diethylamino)benzoato-
\k^2^O,O']dirhodium(II)(Rh---Rh) benzonitrile disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                98.641(6)
_cell_angle_beta                 90.781(6)
_cell_angle_gamma                99.424(6)
_cell_formula_units_Z            1
_cell_length_a                   10.049(4)
_cell_length_b                   12.752(6)
_cell_length_c                   13.479(6)
_cell_measurement_reflns_used    3948
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     1683.3(13)
_computing_cell_refinement       CrystalClear
_computing_data_collection
;
CrystalClear (Molecular Structure Corporation & Rigaku, 2001)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation & Rigaku, 2004)
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and TEXSAN'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0927
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13963
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.710
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         7660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0391P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                5661
_reflns_number_total             7660
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3029.cif
_cod_data_source_block           I
_cod_database_code               2015550
_cod_database_fobs_code          2015550