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_7035115
_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            'C90 H112 Cl4 F12 Ir6 N4 O23 S8'
_chemical_formula_weight         3397.31
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 97.805(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9252(13)
_cell_length_b                   26.276(3)
_cell_length_c                   15.7341(15)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.66
_cell_measurement_theta_min      2.40
_cell_volume                     5703.8(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 0.995
_diffrn_measured_fraction_theta_max 0.994
_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  0.0397
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38726
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.725
_diffrn_reflns_theta_min         1.476
_exptl_absorpt_coefficient_mu    7.298
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_description       block
_exptl_crystal_F_000             3260
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.260
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvents (one triflate anion and half of one 
 diethyl ether molecule) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         3.704
_refine_diff_density_min         -2.855
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         12030
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1259P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1848
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8835
_reflns_number_total             12030
_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_original_cell_volume        5703.8(9)
_cod_database_code               7035115
_audit_block_doi                 10.5517/cc142s22
_shelx_estimated_absorpt_t_min   0.150
_shelx_estimated_absorpt_t_max   0.253
_shelxl_version_number           2013-2
_shelx_res_checksum              13190