Half-sandwich rhodium and iridium metallamacrocycles constructed via C-H activation.
Lin, Lin; Zhang, Ying-Ying; Lin, Yue-Jian; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 45 (2016) 7014–7021; doi:10.1039/c5dt04777c

data_7038741
_publ_section_title
;
 Half-sandwich rhodium and iridium metallamacrocycles constructed via C-H
 activation.
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7014
_journal_page_last               7021
_journal_paper_doi               10.1039/c5dt04777c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C92 H114 Cl8 F12 Ir4 N6 O20 S4'
_chemical_formula_weight         3032.53
_chemical_name_systematic
; 
 ? 
;
_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
_audit_update_record
;
2016-03-07 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.963(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.973(3)
_cell_length_b                   15.042(2)
_cell_length_c                   36.067(5)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.15
_cell_volume                     11131(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.996
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            37332
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.154
_exptl_absorpt_coefficient_mu    5.120
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_description       prism
_exptl_crystal_F_000             5936
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 sovlents (one dichloromethane and two methanol molecules) 
 which could not be restrained properly. Therefore, SQUEEZE 
 algorithm were used to omit them. 
;
_refine_diff_density_max         5.875
_refine_diff_density_min         -4.757
_refine_diff_density_rms         0.266
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         12104
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+617.9258P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9573
_reflns_number_total             12104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04777c2.cif
_cod_data_source_block           3cs
_cod_depositor_comments
'Adding full bibliography for 7038734--7038741.cif.'
_cod_database_code               7038741
_shelx_estimated_absorpt_t_min   0.656
_shelx_estimated_absorpt_t_max   0.862
_shelxl_version_number           2013-2
_shelx_res_checksum              83969