Photochemical Modification of Carbene-Based Metallacycles: A Facile Route to Polycarbene Complexes and Their Derivatives
Wang, Chun-Xiang; Gao, Yang; Deng, Yu-Xin; Lin, Yue-Jian; Han, Ying-Feng; Jin, Guo-Xin; Organometallics 34 (2015) 5801–; doi:10.1021/acs.organomet.5b00977

data_4088268
_publ_section_title
;
 Photochemical Modification of Carbene-Based Metallacycles: A Facile Route
 to Polycarbene Complexes and Their Derivatives
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              5801
_journal_paper_doi               10.1021/acs.organomet.5b00977
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C68 H66 F24 N10 P4'
_chemical_formula_weight         1603.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                79.298(4)
_cell_angle_beta                 72.394(3)
_cell_angle_gamma                65.183(4)
_cell_formula_units_Z            1
_cell_length_a                   11.0245(4)
_cell_length_b                   12.2969(6)
_cell_length_c                   15.1731(6)
_cell_measurement_reflns_used    4352
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.8150
_cell_measurement_theta_min      4.5330
_cell_volume                     1775.46(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12870
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.992
_diffrn_reflns_theta_min         3.970
_exptl_absorpt_coefficient_mu    1.992
_exptl_absorpt_correction_T_max  0.753
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       sheet
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_platon_squeeze_details
; 
 In asymmetric unit of this data, there were disordered 
 anion and solvent (one hexafluorophosphate anion and one 
 acetonitrile molecule) which could not be restrained 
 properly. Therefore, SQUEEZE algorithm was used to omit 
 them. 
;
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.1385P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2201
_refine_ls_wR_factor_ref         0.2378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4471
_reflns_number_total             6462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00977_si_002.cif
_cod_data_source_block           H4-(3)[PF6]4
_cod_original_cell_volume        1775.46(15)
_cod_database_code               4088268
_shelx_estimated_absorpt_t_min   0.796
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2013-2
_shelx_res_checksum              28715
_shelx_hkl_checksum              94682