A Convenient Access to N-Phosphonio-Substituted NHC Metal Complexes [M = Ag(I), Rh(I), Pd(II)]
CANAC, Yves; Lugan, Noël; Benaissa, Idir; Taakili, Rachid; Dalton Trans.  (2017) –; doi:10.1039/C7DT02759A

data_7044108
_publ_section_title
;
 A Convenient Access to N-Phosphonio-Substituted NHC Metal Complexes [M =
 Ag(I), Rh(I), Pd(II)]
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02759A
_journal_year                    2017
_chemical_formula_moiety         '2(Br), C33 H37 N2 P'
_chemical_formula_sum            'C33 H37 Br2 N2 P'
_chemical_formula_weight         652.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-01T14:29:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2017-06-26 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                108.122(2)
_cell_angle_beta                 100.266(2)
_cell_angle_gamma                98.136(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6755(2)
_cell_length_b                   12.7591(3)
_cell_length_c                   13.7838(3)
_cell_measurement_reflns_used    11178
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.5140
_cell_measurement_theta_min      3.7120
_cell_volume                     1555.63(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30779
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.001
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.681
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.503
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         6356
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.05
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.7464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0652
_reflns_Friedel_coverage         0
_reflns_number_gt                5498
_reflns_number_total             6356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02759a2.cif
_cod_data_source_block           3Br2
_cod_original_cell_volume        1555.63(6)
_cod_database_code               7044108
_shelx_res_checksum              82385