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_7038736
_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            'C82 H112 F6 N6 O20 Rh4 S2'
_chemical_formula_weight         2091.53
_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   mixed
_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                 109.8460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   35.819(2)
_cell_length_b                   14.2489(9)
_cell_length_c                   19.1425(13)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.26
_cell_volume                     9189.7(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 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30406
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_min         1.209
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_description       prism
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
 In asymmetric unit of this data, there were disordered 
 solvents (three water and one methanol molecules) which 
 could not be restrained properly. Therefore, SQUEEZE 
 algorithm was used to omit them. 
;
_refine_diff_density_max         4.560
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         9331
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0890P)^2^+37.3102P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1488
_refine_ls_wR_factor_ref         0.1565
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7633
_reflns_number_total             9331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04777c2.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7038734--7038741.cif.'
_cod_database_code               7038736
_shelx_estimated_absorpt_t_min   0.865
_shelx_estimated_absorpt_t_max   0.944
_shelxl_version_number           2013-2
_shelx_res_checksum              12170