Preparation, Crystal Structure, and Unusually Facile Redox Chemistry of a Macrocyclic Nitrosylrhodium Complex
Kathleen E. Kristian; Wenjing Song; Arkady Ellern; Ilia A. Guzei; Andreja Bakac; Inorganic Chemistry 49 (2010) 7182–7187; doi:10.1021/ic101236x

data_4316199
_publ_section_title
;
 Preparation, Crystal Structure, and Unusually Facile Redox Chemistry of a
 Macrocyclic Nitrosylrhodium Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7182
_journal_page_last               7187
_journal_paper_doi               10.1021/ic101236x
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C16 H38.11 Cl2 N4.95 O10 Rh'
_chemical_formula_sum            'C16 H38.11 Cl2 N4.95 O10 Rh'
_chemical_formula_weight         633.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 102.78(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.965(3)
_cell_length_b                   15.393(4)
_cell_length_c                   10.327(4)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      69.4723
_cell_measurement_theta_min      5.2486
_cell_volume                     1234.8(7)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      102(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.50\% \w and 0.5 \% \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0125
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14684
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         5.25
_exptl_absorpt_coefficient_mu    8.121
_exptl_absorpt_correction_T_max  0.5627
_exptl_absorpt_correction_T_min  0.2935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             655
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.630
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2253
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+4.4713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1337
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                2244
_reflns_number_total             2253
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101236x_si_002_1.cif
_cod_data_source_block           bakac01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1234.8(6)
_cod_original_sg_symbol_Hall     '-P 2ybc     '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4316199