Unexpected formation and structural characterisation of a novel rhodium B12 analogue
Bröring, Martin; Cónsul Tejero, Esther; Pfister, Andreas; Brandt, Carsten D.; Pérez Torrente, Jesés J.; Chemical Communications  (2002) 3058–3059; doi:10.1039/b208935c

data_7114184
_publ_section_title
;
 Unexpected formation and structural characterisation of a novel rhodium
 B12 analogue
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              3058
_journal_page_last               3059
_journal_paper_doi               10.1039/b208935c
_journal_year                    2002
_chemical_formula_sum            'C38 H51 Cl6 N4 Rh'
_chemical_formula_weight         879.44
_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                90.0000(10)
_cell_angle_beta                 115.9660(10)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            4
_cell_length_a                   14.4846(11)
_cell_length_b                   20.5801(15)
_cell_length_c                   15.9102(11)
_cell_measurement_reflns_used    8536
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.993
_cell_measurement_theta_min      2.438
_cell_volume                     4264.0(5)
_computing_cell_refinement       'SAINT-NT V5/6.0'
_computing_data_collection       'SMART-NT V5.6'
_computing_data_reduction        'SAINT-NT V5/6.0'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex with D8-Goniometer'
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50208
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS2.0 (Sheldrick 2000)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.610
_refine_diff_density_min         -0.971
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         7808
_refine_ls_number_restraints     403
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0961
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0871P)^2^+14.2746P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2296
_refine_ls_wR_factor_ref         0.2402
_reflns_number_gt                6447
_reflns_number_total             7808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208935c.txt
_cod_data_source_block           ec1cb
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114184