A stepwise assembly of a molecular box from 16-electron half-sandwich precursors [Cp*M(pdt)] (M = Rh, Ir).
Liu, Jing-Jing; Lin, Yue-Jian; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 44 (2015) 10281–10288; doi:10.1039/c5dt01061f

data_7035117
_publ_section_title
;
 A stepwise assembly of a molecular box from 16-electron half-sandwich
 precursors [Cp*M(pdt)] (M = Rh, Ir).
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10281
_journal_page_last               10288
_journal_paper_doi               10.1039/c5dt01061f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C52 H75 Ag F3 N6 O6 Rh3 S7'
_chemical_formula_weight         1578.20
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-01-24 deposited with the CCDC.
2015-04-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.2150(14)
_cell_length_b                   16.4859(10)
_cell_length_c                   28.9810(17)
_cell_measurement_reflns_used    9570
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.47
_cell_volume                     12047.2(12)
_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      193(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  0.0649
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            57878
_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         26.602
_diffrn_reflns_theta_min         1.405
_exptl_absorpt_coefficient_mu    1.432
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             6384
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.110
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvents (one triflate anion, two diethyl ether 
 and one methanol molecules) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         12532
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0971P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7434
_reflns_number_total             12532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01061f2.cif
_cod_data_source_block           complex
_cod_depositor_comments
'Adding full bibliography for 7035112--7035117.cif.'
_cod_database_code               7035117
_audit_block_doi                 10.5517/cc142s44
_shelx_estimated_absorpt_t_min   0.725
_shelx_estimated_absorpt_t_max   0.858
_shelxl_version_number           2013-2
_shelx_res_checksum              28277