Construction of tetranuclear metallacycles based on half-sandwich Ir, Rh fragments and pyridyl-substituted ligands with different coordinate vectors.
Fan, Qi-Jia; Zhang, Wen-Ying; Lin, Yue-Jian; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 45 (2016) 4534–4540; doi:10.1039/c6dt00171h

data_7038177
_publ_section_title
;
 Construction of tetranuclear metallacycles based on half-sandwich Ir, Rh
 fragments and pyridyl-substituted ligands with different coordinate
 vectors.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4534
_journal_page_last               4540
_journal_paper_doi               10.1039/c6dt00171h
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C76 H104 F12 Ir4 N12 O20 S4'
_chemical_formula_weight         2630.75
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-01-25 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   20.111(2)
_cell_length_b                   20.111(2)
_cell_length_c                   12.1229(19)
_cell_measurement_reflns_used    6480
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.21
_cell_volume                     4903.1(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0821
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            33333
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.437
_diffrn_reflns_theta_min         1.432
_exptl_absorpt_coefficient_mu    5.587
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       rod
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvents (half of a diethyl ether and a quarter of a water 
 molecule) which could not be restrained properly. 
 Therefore, SQUEEZE algorithm was used to omit them. 
;
_refine_diff_density_max         2.639
_refine_diff_density_min         -1.727
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.941
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5548
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0531
_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^)+(0.0912P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1420
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2940
_reflns_number_total             5548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00171h1.cif
_cod_data_source_block           4a
_cod_depositor_comments
'Adding full bibliography for 7038175--7038178.cif.'
_cod_original_cell_volume        4903.4(13)
_cod_database_code               7038177
_shelx_estimated_absorpt_t_min   0.213
_shelx_estimated_absorpt_t_max   0.768
_shelxl_version_number           2013-2
_shelx_res_checksum              11683