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_7123984
_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         '2(C72 H71 As B F15 N4 P),C6 H5 Cl'
_chemical_formula_sum            'C75 H73.5 As B Cl0.5 F15 N4 P'
_chemical_formula_weight         1450.30
_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-2018/3
_audit_update_record
;
2019-07-23 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                105.543(4)
_cell_angle_beta                 90.831(4)
_cell_angle_gamma                112.950(6)
_cell_formula_units_Z            2
_cell_length_a                   12.4926(8)
_cell_length_b                   15.7024(10)
_cell_length_c                   20.2821(8)
_cell_measurement_reflns_used    9376
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.6580
_cell_measurement_theta_min      3.3410
_cell_volume                     3497.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)'
_computing_publication_material
'OLEX2 v1.2 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'
_computing_structure_refinement
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122)'
_computing_structure_solution
'SHELXT-2014/5 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36387
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         2.282
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.789
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.21a (Rigaku Oxford Diffraction, 2018)
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            green
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       needle
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.032
_refine_diff_density_max         1.391
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         12081
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0938
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.033
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1211P)^2^+1.3233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8718
_reflns_number_total             12081
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05739k3.cif
_cod_data_source_block           ph46ph
_cod_original_formula_sum        'C75 H73.50 As B Cl0.50 F15 N4 P'
_cod_database_code               7123984
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.745
_shelx_estimated_absorpt_t_max   0.945
_shelx_res_checksum              24580