Coordination chemistry of a low-coordinate non-metal element: the case of electrophilic terminal phosphinidene complexes.
Villalba Franco, José Manuel; Schnakenburg, Gregor; Espinosa Ferao, Arturo; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 45 (2016) 13951–13956; doi:10.1039/c6dt02909d

data_7040330
_publ_section_title
;
 Coordination chemistry of a low-coordinate non-metal element: the case of
 electrophilic terminal phosphinidene complexes.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13951
_journal_page_last               13956
_journal_paper_doi               10.1039/c6dt02909d
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C32 H29 N2 O6 P W'
_chemical_formula_sum            'C32 H29 N2 O6 P W'
_chemical_formula_weight         752.39
_chemical_name_systematic        JMV-460
_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_date             2015-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-03 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                96.245(3)
_cell_angle_beta                 104.796(3)
_cell_angle_gamma                103.755(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5330(5)
_cell_length_b                   10.1180(5)
_cell_length_c                   17.1899(8)
_cell_measurement_reflns_used    4748
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.970
_cell_measurement_theta_min      2.857
_cell_volume                     1531.52(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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
_diffrn_detector                 'ApexII detector'
_diffrn_detector_area_resol_mean 8
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.868
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       '\f and \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  0.1137
_diffrn_reflns_av_unetI/netI     0.2368
_diffrn_reflns_Laue_measured_fraction_full 0.868
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10946
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.634
_diffrn_source                   'sealed tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.869
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0964 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.8377.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.986
_refine_diff_density_min         -3.468
_refine_diff_density_rms         0.297
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         4823
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0399P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2918
_reflns_number_total             4823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02909d2.cif
_cod_data_source_block           4051h
_cod_depositor_comments
'Adding full bibliography for 7040329--7040331.cif.'
_cod_original_cell_volume        1531.52(13)
_cod_database_code               7040330
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.861
_shelx_estimated_absorpt_t_min   0.654
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C17) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_olex2_submission_original_sample_id JMV-460
_olex2_submission_special_instructions 'No special instructions were received'