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_7123980
_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 B Cl F15 N4 P2, 0.5(C6 D6)'
_chemical_formula_sum            'C75 H71 B Cl D3 F15 N4 P2'
_chemical_formula_weight         1427.60
_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                99.475(4)
_cell_angle_beta                 93.788(4)
_cell_angle_gamma                109.582(4)
_cell_formula_units_Z            2
_cell_length_a                   13.5450(6)
_cell_length_b                   14.3760(10)
_cell_length_c                   19.5043(8)
_cell_measurement_reflns_used    17925
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.0020
_cell_measurement_theta_min      3.3220
_cell_volume                     3499.3(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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Nova'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            70864
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.204
_diffrn_reflns_theta_min         3.329
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.657
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.951
_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            orange
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1478
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         14515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0854P)^2^+1.6738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1521
_refine_ls_wR_factor_ref         0.1668
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11103
_reflns_number_total             14515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05739k3.cif
_cod_data_source_block           ph08ph
_cod_database_code               7123980
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.563
_shelx_estimated_absorpt_t_max   0.879
_oxdiff_exptl_absorpt_empirical_full_min 0.507
_oxdiff_exptl_absorpt_empirical_full_max 2.155
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              65855