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_4316200
_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 N5 O3 Rh, 2(Cl O4), 2(H2O)'
_chemical_formula_sum            'C16 H42 Cl2 N5 O13 Rh'
_chemical_formula_weight         686.36
_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                90.00
_cell_angle_beta                 94.022(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.627(4)
_cell_length_b                   19.052(7)
_cell_length_c                   13.751(5)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.34
_cell_volume                     2777.2(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      198(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24578
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.8308
_exptl_absorpt_correction_T_min  0.6638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0598P)^2^+4.0950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                5188
_reflns_number_total             6540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101236x_si_002_2.cif
_cod_data_source_block           bak24
_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2777.4(18)
_cod_database_code               4316200