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_4088267
_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            'C74 H75 Ag2 B F10 N9 P'
_chemical_formula_weight         1537.95
_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                83.216(2)
_cell_angle_beta                 75.227(2)
_cell_angle_gamma                73.672(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8068(13)
_cell_length_b                   15.4203(16)
_cell_length_c                   21.207(2)
_cell_measurement_reflns_used    4424
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.09
_cell_measurement_theta_min      2.44
_cell_volume                     3578.3(6)
_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 0.985
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0844
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23523
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         0.994
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.040
_platon_squeeze_details          ' '
_refine_diff_density_max         1.232
_refine_diff_density_min         -1.405
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     901
_refine_ls_number_reflns         13859
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0779
_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^)+(0.1996P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7900
_reflns_number_total             13859
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00977_si_003.cif
_cod_data_source_block           Ag2(4)(PF6)2
_cod_original_cell_volume        3578.3(7)
_cod_database_code               4088267
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.975
_shelxl_version_number           2013-2
_shelx_res_checksum              32697
_shelx_hkl_checksum              98821