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_7121323
_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 N2 P2'
_chemical_formula_sum            'C29 H44 N2 P2'
_chemical_formula_weight         482.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2017-11-06 deposited with the CCDC.
2018-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.6105(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7612(4)
_cell_length_b                   24.4504(10)
_cell_length_c                   14.3595(6)
_cell_measurement_reflns_used    9536
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.26
_cell_measurement_theta_min      2.43
_cell_volume                     3416.0(2)
_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      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_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 and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0128
_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       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            122745
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.314
_diffrn_reflns_theta_min         2.191
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.7286
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0828 before and 0.0522 after correction. The Ratio of minimum to maximum transmission is 0.9797. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.938
_exptl_crystal_description       needle
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+2.3600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5639
_reflns_number_total             6214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00899j2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 7121321--7121324.cif.'
_cod_database_code               7121323
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C10)=Sof(H10A)=Sof(H10B)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(1)
 Fixed Sof: H12C(0.5) H12D(0.5) H12A(0.5) H12B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C12(H12C,H12D), C12(H12A,H12B), C11(H11A,H11B), C10(H10A,H10B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C6(H6), C4(H4), C17(H17)
3.c Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C29(H29A,H29B,H29C), C21(H21A,H21B,H21C), C19(H19A,H19B,
 H19C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C28(H28A,
 H28B,H28C), C20(H20A,H20B,H20C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C),
 C27(H27A,H27B,H27C)
;
_shelx_res_checksum              48092
_shelx_fab_checksum              92311
_olex2_submission_special_instructions 'No special instructions were received'