Synthesis, Characterization, and Properties of Half-Sandwich Iridium/Rhodium-Based Metallarectangles
Zhang, Wen-Ying; Han, Ying-Feng; Weng, Lin-Hong; Jin, Guo-Xin; Organometallics 33 (2014) 3091–; doi:10.1021/om500338w

data_4083561
_publ_section_title
;
 Synthesis, Characterization, and Properties of Half-Sandwich
 Iridium/Rhodium-Based Metallarectangles
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3091
_journal_paper_doi               10.1021/om500338w
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C228 H172 Cl4 F12 Ir4 N8 O30 S4'
_chemical_formula_weight         4770.57
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 116.899(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.192(3)
_cell_length_b                   29.161(4)
_cell_length_c                   19.192(3)
_cell_measurement_reflns_used    6217
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      24.32
_cell_measurement_theta_min      2.41
_cell_volume                     9579(3)
_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      203(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.996
_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  0.0752
_diffrn_reflns_av_unetI/netI     0.0965
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47931
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.245
_exptl_absorpt_coefficient_mu    2.959
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       prism
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         5.574
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1363
_refine_ls_number_reflns         16825
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0941P)^2^+53.2107P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10713
_reflns_number_total             16825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500338w_si_002.cif
_cod_data_source_block           4a
_cod_depositor_comments          'Adding full bibliography for 4083561.cif.'
_cod_original_cell_volume        9579(2)
_cod_database_code               4083561
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.798
_shelxl_version_number           2013-2
_shelx_res_checksum              51148
_shelx_hkl_checksum              14645