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_2015551
_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 (C7 H4 N O4)4 (C2 H4 O) (C5 H5 N)] , C H2 Cl2'
_chemical_formula_moiety         'C34 H25 N5 O17 Rh2 , C H2 Cl2'
_chemical_formula_sum            'C35 H27 Cl2 N5 O17 Rh2'
_chemical_formula_weight         1066.34
_chemical_name_systematic
;
(methanol)tetrakis(\m-<i>p</i>-nitrobenzoato-
\k^2^O,O')(pyridine)dirhodium(II)(Rh---Rh) dichloromethane solvate,
[Rh~2~(C~7~H~4~NO~4~)~4~(C~2~H~4~O)(C~5~H~5~N)].CH~2~Cl~2~
;
_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                96.55(3)
_cell_angle_beta                 109.420(10)
_cell_angle_gamma                118.430(10)
_cell_formula_units_Z            2
_cell_length_a                   12.750(6)
_cell_length_b                   13.290(4)
_cell_length_c                   14.773(5)
_cell_measurement_reflns_used    5195
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     1961.0(14)
_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      113(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16189
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.819
_refine_diff_density_min         -1.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0533P)^2^+2.6928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                6931
_reflns_number_total             8932
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3029.cif
_cod_data_source_block           II
_cod_original_cell_volume        1961.0(13)
_cod_database_code               2015551
_cod_database_fobs_code          2015551