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_7032646
_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 Ir4 N8 O8, 4(C F3 O3 S), 3(C H4 O), (C4 H10 O), 4(H2 O)'
_chemical_formula_sum            'C95 H138 B20 F12 Ir4 N8 O28 S4'
_chemical_formula_weight         3181.37
_chemical_name_systematic        3a
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.667(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7262(18)
_cell_length_b                   25.171(3)
_cell_length_c                   27.215(3)
_cell_measurement_reflns_used    6273
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.40
_cell_measurement_theta_min      2.40
_cell_volume                     12084(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 0.972
_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  0.1155
_diffrn_reflns_av_unetI/netI     0.1425
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            72543
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.154
_exptl_absorpt_coefficient_mu    4.552
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_description       sheet
_exptl_crystal_F_000             6272
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.040
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvents (three methanol and one diethyl ether molecules) 
 which could not be restrained properly. Therefore, SQUEEZE 
 algorithm were used to omit them. 
;
_refine_diff_density_max         2.062
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1495
_refine_ls_number_reflns         21257
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0633
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0876P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11100
_reflns_number_total             21257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02495h1.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 7032645--7032650.cif.'
_cod_original_cell_volume        12083(2)
_cod_database_code               7032646
_shelx_estimated_absorpt_t_min   0.434
_shelx_estimated_absorpt_t_max   0.839
_shelxl_version_number           2013-2
_shelx_res_checksum              84204