Well-Defined, Shelf-Stable (NHC)Ag(CF2H) Complexes for Difluoromethylation
Gu, Yang; Chang, Dalu; Leng, Xuebing; Gu, Yucheng; Shen, Qilong; Organometallics 34 (2015) 3065–; doi:10.1021/acs.organomet.5b00350

data_4085936
_publ_section_title
;
 Well-Defined, Shelf-Stable (NHC)Ag(CF2H) Complexes for
 Difluoromethylation
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3065
_journal_paper_doi               10.1021/acs.organomet.5b00350
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C28 H39 Ag F2 N2'
_chemical_formula_weight         549.48
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.785(5)
_cell_length_b                   11.325(3)
_cell_length_c                   12.641(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2832.4(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16587
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.059
_exptl_absorpt_coefficient_mu    0.741
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.022
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
; 
 Flack x determined using 1894 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.540(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5523
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.898
_reflns_friedel_fraction_full    0.990
_reflns_friedel_fraction_max     0.988
_reflns_number_gt                4469
_reflns_number_total             5523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00350_si_002.cif
_cod_data_source_block           cd213195
_cod_depositor_comments
'Adding full bibliography for 4085936--4085937.cif.'
_cod_original_cell_volume        2832.3(12)
_cod_database_code               4085936
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.930
_shelxl_version_number           2013-4
_shelx_res_checksum              97864
_shelx_hkl_checksum              48998