From the parent phosphinidene-carbene adduct NHC[double bond, length as m-dash]PH to cationic P4-rings and P2-cycloaddition products.
Beil, Andreas; Gilliard, Robert J.; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 45 (2016) 2044–2052; doi:10.1039/c5dt03014e

data_7036651
_publ_section_title
;
 From the parent phosphinidene-carbene adduct NHC[double bond, length as
 m-dash]PH to cationic P4-rings and P2-cycloaddition products.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2044
_journal_page_last               2052
_journal_paper_doi               10.1039/c5dt03014e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'Cl4 Ga, C39 H60 N3 P2'
_chemical_formula_sum            'C39 H60 Cl4 Ga N3 P2'
_chemical_formula_weight         844.36
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-07-28 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.0720(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7703(2)
_cell_length_b                   15.0762(3)
_cell_length_c                   27.5758(5)
_cell_measurement_reflns_used    9944
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.64
_cell_measurement_theta_min      2.63
_cell_volume                     4394.28(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.33
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART Apex2'
_diffrn_measurement_method       '\w and \f 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  0.0272
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            34737
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.022
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_T_max  0.9137
_exptl_absorpt_correction_T_min  0.8431
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0544 before and 0.0395 after correction.
The Ratio of minimum to maximum transmission is 0.9227.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear greenish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       block
_exptl_crystal_F_000             1776
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DME/hexane'
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0521P)^2^+2.3029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7220
_reflns_number_total             8936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03014e2.cif
_cod_data_source_block           4b
_cod_depositor_comments
'Adding full bibliography for 7036646--7036654.cif.'
_cod_database_code               7036651
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.761
_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(C12B) = Uanis(C12A)
3. Others
 Sof(H10A)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(H12C)=1-FVAR(1)
 Sof(H10)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C22(H22), C25(H25), C28(H28), C10(H10A), C10(H10), C31(H31)
4.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C37(H37A,H37B)
4.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C19(H19), C3(H3), C2(H2), C6(H6), C18(H18), C8(H8), C7(H7)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C15(H15A,H15B,H15C), C23(H23A,H23B,
 H23C), C38(H38A,H38B,H38C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C), C11(H11A,H11B,H11C),
 C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C12B(H12A,H12B,H12C), C12A(H12D,H12E,
 H12F)
;
_shelx_res_checksum              20832
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'