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_7123982
_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 B F15 N4 P2), C4 H8 O'
_chemical_formula_sum            'C74 H75 B F15 N4 O0.5 P2'
_chemical_formula_weight         1386.13
_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                105.855(2)
_cell_angle_beta                 90.306(2)
_cell_angle_gamma                112.409(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5253(2)
_cell_length_b                   15.4459(2)
_cell_length_c                   20.2657(2)
_cell_measurement_reflns_used    82449
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      77.4590
_cell_measurement_theta_min      3.2590
_cell_volume                     3460.21(11)
_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 1.000
_diffrn_measured_fraction_theta_max 0.989
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            144778
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.620
_diffrn_reflns_theta_min         2.284
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.399
_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            'red-green dichroic'
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1442
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         14569
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0641P)^2^+2.1893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13627
_reflns_number_total             14569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc05739k3.cif
_cod_data_source_block           ph40ph
_cod_original_cell_volume        3460.20(10)
_cod_original_formula_sum        'C74 H75 B F15 N4 O0.50 P2'
_cod_database_code               7123982
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.695
_shelx_estimated_absorpt_t_max   0.830
_shelx_res_checksum              31781