Construction of iridium and rhodium cyclometalated macrocycles based on p-carborane and N,N'-donor bridging ligands.
Shen, Xu-Yu; Zhang, Long; Lin, Yue-Jian; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 43 (2014) 17200–17208; doi:10.1039/c4dt02495h

data_7032648
_publ_section_title
;
 Construction of iridium and rhodium cyclometalated macrocycles based on
 p-carborane and N,N'-donor bridging ligands.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17200
_journal_page_last               17208
_journal_paper_doi               10.1039/c4dt02495h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety
'C84 H108 B20 N8 O8 Rh4, 4(C F3 O3 S), 2(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C90 H120 B20 F12 N8 O24 Rh4 S4'
_chemical_formula_weight         2682.01
_chemical_name_systematic        3b
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.947(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5981(19)
_cell_length_b                   40.947(5)
_cell_length_c                   16.9617(18)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.27
_cell_volume                     12480(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0625
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            39953
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.010
_diffrn_reflns_theta_min         0.995
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvents (one methanol and one water molecules). Therefore, 
 SQUEEZE algorithm was used to omit them. 
;
_refine_diff_density_max         2.790
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         12258
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.1184
_refine_ls_R_factor_gt           0.0870
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1990P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2488
_refine_ls_wR_factor_ref         0.2797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8384
_reflns_number_total             12258
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02495h1.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 7032645--7032650.cif.'
_cod_database_code               7032648
_shelx_estimated_absorpt_t_min   0.912
_shelx_estimated_absorpt_t_max   0.936
_shelxl_version_number           2013-2
_shelx_res_checksum              90063