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_4122908
_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            'C54.5 H74.5 B4 F16 Ir2 N8.5 O2 S4'
_chemical_formula_weight         1740.60
_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                96.441(2)
_cell_angle_beta                 97.220(2)
_cell_angle_gamma                106.428(2)
_cell_formula_units_Z            4
_cell_length_a                   11.1337(10)
_cell_length_b                   18.7761(17)
_cell_length_c                   33.960(3)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.23
_cell_measurement_theta_min      2.29
_cell_volume                     6673.5(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 0.986
_diffrn_measured_fraction_theta_max 0.987
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0999
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43415
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.010
_diffrn_reflns_theta_min         1.211
_exptl_absorpt_coefficient_mu    4.201
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       sheet
_exptl_crystal_F_000             3436
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.020
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disorder anions 
 and solvents (two tetrafluoroborate anions, one DMF, two 
 methanol and one water molecules) which could not be 
 restrained properly. Therefore, SQUEEZE algorithm was used 
 to omit them. 
;
_refine_diff_density_max         2.211
_refine_diff_density_min         -1.901
_refine_diff_density_rms         0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1475
_refine_ls_number_reflns         25922
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1467P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16647
_reflns_number_total             25922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja508543y_si_001.cif
_cod_data_source_block           1a(BF4)4
_cod_original_formula_sum        'C54.50 H74.50 B4 F16 Ir2 N8.50 O2 S4'
_cod_database_code               4122908
_shelx_estimated_absorpt_t_min   0.519
_shelx_estimated_absorpt_t_max   0.921
_shelxl_version_number           2013-2
_shelx_res_checksum              61219
_shelx_hkl_checksum              68467