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_7036652
_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, C35 H52 N3 P2'
_chemical_formula_sum            'C35 H52 Cl4 Ga N3 P2'
_chemical_formula_weight         788.25
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-28
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.036(3)
_cell_length_b                   18.337(2)
_cell_length_c                   21.409(3)
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.09
_cell_measurement_theta_min      2.32
_cell_volume                     7865.7(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SAINT'
_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 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD'
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55921
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.187
_diffrn_reflns_theta_min         1.781
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.575
_diffrn_source_target            Mo
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0449 before and 0.0401 after correction.
The Ratio of minimum to maximum transmission is 0.9174.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DME/hexane'
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.264
_refine_diff_density_max         0.849
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         10588
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0410
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1428
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9059
_reflns_number_total             10588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03014e2.cif
_cod_data_source_block           4c
_cod_depositor_comments
'Adding full bibliography for 7036646--7036654.cif.'
_cod_original_cell_volume        7865.6(18)
_cod_database_code               7036652
_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
Cl1X \\sim Cl1Y: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
Cl2X \\sim Cl2Y: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(Cl2Y) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Others
 Sof(GaY)=Sof(Cl4Y)=Sof(Cl3Y)=Sof(Cl2Y)=Sof(Cl1Y)=1-FVAR(1)
 Sof(GaX)=Sof(Cl4X)=Sof(Cl3X)=Sof(Cl2X)=Sof(Cl1X)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C22(H22), C10(H10), C13(H13), C25(H25)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b), C33(H33a,H33b)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C20(H20), C18(H18), C6(H6), C7(H7), C19(H19), C8(H8)
4.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C24(H24a,H24b,H24c), C34(H34a,H34b,H34c), C29(H29a,H29b,
 H29c), C12(H12a,H12b,H12c), C28(H28a,H28b,H28c), C23(H23a,H23b,H23c), C35(H35a,
 H35b,H35c), C27(H27a,H27b,H27c), C26(H26a,H26b,H26c), C14(H14a,H14b,H14c),
 C15(H15a,H15b,H15c)
;
_shelx_res_checksum              77678
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'