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_7032649
_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
'C92 H124 B20 N8 O8 Rh4, 4(C F3 O3 S), 6(C H4 O), 8(H2 O)'
_chemical_formula_sum            'C102 H164 B20 F12 N8 O34 Rh4 S4'
_chemical_formula_weight         3030.48
_chemical_name_systematic        4b
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 102.403(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.1486(14)
_cell_length_b                   18.488(2)
_cell_length_c                   30.333(3)
_cell_measurement_reflns_used    6927
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.94
_cell_measurement_theta_min      2.16
_cell_volume                     7201.6(13)
_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 0.993
_diffrn_measured_fraction_theta_max 0.994
_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  0.0776
_diffrn_reflns_av_unetI/netI     0.1063
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            49815
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.587
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvents (three methanol and two water molecules) which 
 could not be restrained properly. Therefore, SQUEEZE 
 algorithm was used to omit them. 
;
_refine_diff_density_max         2.532
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         15616
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1591
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1868P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2777
_refine_ls_wR_factor_ref         0.3085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8233
_reflns_number_total             15616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02495h1.cif
_cod_data_source_block           4b
_cod_depositor_comments
'Adding full bibliography for 7032645--7032650.cif.'
_cod_original_cell_volume        7201.7(13)
_cod_database_code               7032649
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.916
_shelxl_version_number           2013-2
_shelx_res_checksum              2763