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_4122918
_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            'C77 H114 Ir2 N18 O19 S6'
_chemical_formula_weight         2172.62
_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                86.9220(10)
_cell_angle_beta                 72.937(2)
_cell_angle_gamma                83.271(2)
_cell_formula_units_Z            2
_cell_length_a                   14.7490(12)
_cell_length_b                   15.4204(13)
_cell_length_c                   22.4129(18)
_cell_measurement_reflns_used    4918
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.61
_cell_measurement_theta_min      2.29
_cell_volume                     4838.5(7)
_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 0.988
_diffrn_measured_fraction_theta_max 0.983
_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  0.0506
_diffrn_reflns_av_unetI/netI     0.1266
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36551
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.791
_diffrn_reflns_theta_min         0.951
_exptl_absorpt_coefficient_mu    2.948
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anions and solvents (one nitrate anion, two methanol and 
 two water molecules) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm were used to omit 
 them. 
;
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.247
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         22517
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0983P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12984
_reflns_number_total             22517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508543y_si_001.cif
_cod_data_source_block           8(NO3)3
_cod_database_code               4122918
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.891
_shelxl_version_number           2013-2
_shelx_res_checksum              51494
_shelx_hkl_checksum              32276