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_7038738
_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            'C88 H130 F12 N6 O30 Rh4 S4'
_chemical_formula_weight         2519.85
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-02-01 deposited with the CCDC.
2016-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.280(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.337(5)
_cell_length_b                   14.113(2)
_cell_length_c                   14.318(2)
_cell_measurement_reflns_used    6090
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.78
_cell_measurement_theta_min      2.43
_cell_volume                     5485.5(14)
_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 0.990
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18510
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.604
_diffrn_reflns_theta_min         1.500
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 solvents (four methanol and three water molecules) which 
 could not be restrained properly. Therefore,  SQUEEZE 
 algorithm was used to omit them. 
;
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
; 
 Flack x determined using 3437 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         11168
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0904P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1324
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.961
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                8574
_reflns_number_total             11168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04777c2.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7038734--7038741.cif.'
_cod_original_cell_volume        5485.3(16)
_cod_database_code               7038738
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.928
_shelxl_version_number           2013-2
_shelx_res_checksum              51775