Phosphaalkene-substituted organo-group 15 compounds: synthesis and characterisation of (NHC)P-EtBu<sub>2</sub> (E = P, As, Sb and Bi).
Balmer, Markus; Gottschling, Hannah; von Hänisch, Carsten; Chemical communications (Cambridge, England) 54 (2018) 2659–2661; doi:10.1039/c8cc00899j

data_7121324
_publ_section_title
;
 Phosphaalkene-substituted organo-group 15 compounds: synthesis and
 characterisation of (NHC)P-EtBu<sub>2</sub> (E = P, As, Sb and Bi).
;
_journal_issue                   21
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2659
_journal_page_last               2661
_journal_paper_doi               10.1039/c8cc00899j
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C29 H44 As N2 P, C7 H8'
_chemical_formula_sum            'C36 H52 As N2 P'
_chemical_formula_weight         618.68
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-11-06 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                88.700(2)
_cell_angle_beta                 82.678(3)
_cell_angle_gamma                71.476(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4313(5)
_cell_length_b                   11.7613(7)
_cell_length_c                   16.5108(9)
_cell_measurement_reflns_used    9756
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      26.718
_cell_measurement_theta_min      2.44
_cell_volume                     1722.09(17)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.783
_diffrn_reflns_theta_min         2.229
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.8118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1260 before and 0.0398 after correction. The Ratio of minimum to maximum transmission is 0.8747. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.151
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         7311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0310P)^2^+0.9630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6681
_reflns_number_total             7311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00899j2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7121321--7121324.cif.'
_cod_database_code               7121324
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.641
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2B) = Uanis(C3B)
3. Others
 Sof(N1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=1-FVAR(1)
 Sof(N1B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=FVAR(1)
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(2)
 Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(3)
 Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H29C)=FVAR(3)
 Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=1-FVAR(4)
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(4)
4.a Secondary CH2 refined with riding coordinates:
 C2B(H2BA,H2BB), C3B(H3BA,H3BB), C2A(H2AA,H2AB), C3A(H3AA,H3AB)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C8(H8), C17(H17), C6(H6), C32(H32), C36(H36), C33(H33), C35(H35),
 C34(H34)
4.c Idealised Me refined as rotating group:
 C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F), C29A(H29A,H29B,H29C), C29B(H29D,
 H29E,H29F), C25A(H25A,H25B,H25C), C24A(H24A,H24B,H24C), C25B(H25D,H25E,H25F),
 C24B(H24D,H24E,H24F), C19(H19A,H19B,H19C), C27(H27A,H27B,H27C), C23(H23A,H23B,
 H23C), C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C21(H21A,
 H21B,H21C), C11(H11A,H11B,H11C), C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'