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_4122917
_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            'C62 H90 F12 Ir2 N8 O18 S8'
_chemical_formula_weight         2104.29
_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   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.866(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3564(10)
_cell_length_b                   27.465(3)
_cell_length_c                   13.0954(12)
_cell_measurement_reflns_used    4970
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.25
_cell_volume                     3947.8(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 0.993
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            28781
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.464
_diffrn_reflns_theta_min         1.483
_exptl_absorpt_coefficient_mu    3.677
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_description       block
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were three 
 disordered methanol molecules which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         1.243
_refine_diff_density_min         -2.344
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         8978
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      0.896
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1135P)^2^+0.7136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6081
_reflns_number_total             8978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508543y_si_001.cif
_cod_data_source_block           7(OTf)4
_cod_original_cell_volume        3947.8(6)
_cod_database_code               4122917
_shelx_estimated_absorpt_t_min   0.710
_shelx_estimated_absorpt_t_max   0.898
_shelxl_version_number           2013-4
_shelx_res_checksum              79301
_shelx_hkl_checksum              37569