H2-Initiated Reversible Switching between Two-Dimensional Metallacycles and Three-Dimensional Cylinders.
Han, Ying-Feng; Zhang, Long; Weng, Lin-Hong; Jin, Guo-Xin; Journal of the American Chemical Society 136 (2014) 14608–; doi:10.1021/ja508543y

data_4122921
_publ_section_title
;
 H2-Initiated Reversible Switching between Two-Dimensional Metallacycles
 and Three-Dimensional Cylinders.
;
_journal_issue                   41
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14608
_journal_paper_doi               10.1021/ja508543y
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C89 H128 F12 Ir2 N12 O17 S10'
_chemical_formula_weight         2571.03
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                80.2970(10)
_cell_angle_beta                 78.4570(10)
_cell_angle_gamma                65.4890(10)
_cell_formula_units_Z            2
_cell_length_a                   15.7876(13)
_cell_length_b                   16.5051(14)
_cell_length_c                   24.296(2)
_cell_measurement_reflns_used    8215
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.29
_cell_volume                     5617.9(8)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39633
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         0.859
_exptl_absorpt_coefficient_mu    2.635
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered
 solvents (two methanol) which could not be restrained
 properly. Therefore, SQUEEZE algorithm was used to omit
 them. 
;
_refine_diff_density_max         3.223
_refine_diff_density_min         -2.054
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1249
_refine_ls_number_reflns         24188
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0675
_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^)+(0.1577P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1919
_refine_ls_wR_factor_ref         0.2340
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15425
_reflns_number_total             24188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508543y_si_001.cif
_cod_data_source_block           10(OTf)4
_cod_original_cell_volume        5618.0(8)
_cod_database_code               4122921
_shelx_estimated_absorpt_t_min   0.634
_shelx_estimated_absorpt_t_max   0.880
_shelxl_version_number           2013-2
_shelx_res_checksum              27479
_shelx_hkl_checksum              40510