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_7038739
_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 H96 Cl8 Ir4 N4 O8'
_chemical_formula_weight         2438.12
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_symmetry_space_group_name_Hall  '-F 2 2'
_symmetry_space_group_name_H-M   'F m m m'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1570(16)
_cell_length_b                   25.995(4)
_cell_length_c                   53.545(8)
_cell_measurement_reflns_used    6969
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.44
_cell_volume                     14138(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -68
_diffrn_reflns_number            25216
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.312
_diffrn_reflns_theta_min         0.761
_exptl_absorpt_coefficient_mu    3.941
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       block
_exptl_crystal_F_000             4736
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.080
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvent molcules (half of a dichloromethane molecule) which 
 could not be restrained properly. Therefore, SQUEEZE 
 algorithm was used to omit it. 
;
_refine_diff_density_max         1.807
_refine_diff_density_min         -1.951
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         4334
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0517
_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^)+(0.1053P)^2^+11.9652P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3301
_reflns_number_total             4334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04777c2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7038734--7038741.cif.'
_cod_original_cell_volume        14137(4)
_cod_database_code               7038739
_shelx_estimated_absorpt_t_min   0.492
_shelx_estimated_absorpt_t_max   0.743
_shelxl_version_number           2013-2
_shelx_res_checksum              26021