Heteroleptic diphosphenes and arsaphosphenes bearing neutral and anionic N-heterocyclic carbenes
Ho, Luong Phong; Zaretzke, Marc-Kevin; Bannenberg, Thomas; Tamm, Matthias; Chemical Communications  (2019) –; doi:10.1039/C9CC05739K

data_7123985
_publ_section_title
;
 Heteroleptic diphosphenes and arsaphosphenes bearing neutral and anionic
 N-heterocyclic carbenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05739K
_journal_year                    2019
_chemical_formula_moiety         'C72 H71 As B Cl F15 N4 P, 0.5(C6 H6)'
_chemical_formula_sum            'C75 H74 As B Cl F15 N4 P'
_chemical_formula_weight         1468.53
_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-2014/7
_audit_update_record
;
2019-07-23 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                99.868(4)
_cell_angle_beta                 93.997(4)
_cell_angle_gamma                108.674(5)
_cell_formula_units_Z            2
_cell_length_a                   13.5035(8)
_cell_length_b                   14.3960(8)
_cell_length_c                   19.4613(8)
_cell_measurement_reflns_used    12579
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.5020
_cell_measurement_theta_min      3.4630
_cell_volume                     3499.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_publication_material
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;
_computing_structure_refinement
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_structure_solution
;
 SHELXT-2014/7 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1297
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            82893
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.706
_diffrn_reflns_theta_min         3.311
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.966
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.986
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       plate
_exptl_crystal_F_000             1514
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.077
_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     899
_refine_ls_number_reflns         14545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0607P)^2^+2.0634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1329
_refine_ls_wR_factor_ref         0.1555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10106
_reflns_number_total             14545
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05739k3.cif
_cod_data_source_block           ph09ph
_cod_database_code               7123985
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.777
_shelx_estimated_absorpt_t_max   0.951
_shelx_res_checksum              17779