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_7032645
_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
'C38 H44 Cl2 Ir2 N4, 2(C F3 O3 S), 2/3(C7 H8), 4/3(C H2 Cl2)'
_chemical_formula_sum            'C46 H52 Cl4.66667 F6 Ir2 N4 O6 S2'
_chemical_formula_weight         1484.87
_chemical_name_systematic        2a
_chemical_properties_physical    Air-sensitive
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.444(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   23.249(3)
_cell_length_b                   20.772(3)
_cell_length_c                   35.211(5)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.44
_cell_volume                     16131(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.992
_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  0.0637
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            57266
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.219
_exptl_absorpt_coefficient_mu    5.324
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_description       prism
_exptl_crystal_F_000             8680
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_platon_squeeze_details
; 
 In asymmetric unit of this data, there was disordered 
 solvent molecule (one dichloromethane) which could not be 
 restrained properly. Therefore, SQUEEZE algorithm was used 
 to omit it. 
;
_refine_diff_density_max         1.787
_refine_diff_density_min         -2.577
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         18388
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0709
_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^)+(0.0755P)^2^+339.5220P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1804
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13264
_reflns_number_total             18388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02495h1.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
Adding full bibliography for 7032645--7032650.cif.

2018-06-04
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C138 H156 Cl14 F18 Ir6 N12 O18 S6'
_cod_original_formula_weight         4454.60
_cod_original_formula_moiety
'3(C38 H44 Cl2 Ir2 N4), 6(C F3 O3 S), 2(C7 H8), 4(C H2 Cl2)'
_cod_original_formula_units_Z            4
_cod_database_code               7032645
_shelx_estimated_absorpt_t_min   0.208
_shelx_estimated_absorpt_t_max   0.646
_shelxl_version_number           2013-2
_shelx_res_checksum              45175