Insertion of phenyl isothiocyanate into a P-P bond of a nickel-substituted bicyclo[1.1.0]tetraphosphabutane.
Pelties, Stefan; Ehlers, Andreas W.; Wolf, Robert; Chemical communications (Cambridge, England) 52 (2016) 6601–6604; doi:10.1039/c6cc01572g

data_7124606
_publ_section_title
;
 Insertion of phenyl isothiocyanate into a P-P bond of a
 nickel-substituted bicyclo[1.1.0]tetraphosphabutane.
;
_journal_issue                   39
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6601
_journal_page_last               6604
_journal_paper_doi               10.1039/c6cc01572g
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C59 H63 N5 Ni2 P4 S, 2(C7 H8)'
_chemical_formula_sum            'C73 H79 N5 Ni2 P4 S'
_chemical_formula_weight         1299.77
_chemical_name_common            '[CpNi(IMes)]2(P4C(S)NPh)](tol)2'
_chemical_name_systematic        2b
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-07 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                104.2274(14)
_cell_angle_beta                 103.1281(14)
_cell_angle_gamma                106.3708(16)
_cell_formula_units_Z            2
_cell_length_a                   12.4533(2)
_cell_length_b                   15.5940(3)
_cell_length_c                   19.3068(3)
_cell_measurement_reflns_used    12410
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      72.9320
_cell_measurement_theta_min      3.9960
_cell_volume                     3305.15(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
  1 omega -112.00  -14.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -37.0000 -120.0000 196

  2 omega  -98.00   -2.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  125.0000  120.0000 192

  3 omega  -67.00   35.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064   37.0000   60.0000 204

  4 omega   33.00  140.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000 -150.0000 214

  5 omega   30.00   60.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   90.0000 60

  6 omega   33.00   67.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  120.0000 68

  7 omega   83.00  158.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000  -30.0000 150

  8 omega   32.00  121.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000   30.0000 178

  9 omega   31.00   69.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -180.0000 76

 10 omega   36.00   67.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -150.0000 62

 11 omega   28.00  134.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000   30.0000 212

 12 omega   32.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  150.0000 66

 13 omega   55.00  121.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000 -150.0000 132

 14 omega   73.00  132.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   90.0000 118

 15 omega   46.00  155.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   15.0000   90.0000 218

 16 omega -119.00   -7.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -77.0000  -30.0000 224

 17 omega -115.00  -11.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -57.0000  150.0000 208

 18 omega -119.00   -7.00   0.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.7064  -77.0000   60.0000 224

 19 omega   77.00  158.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -90.0000 162

 20 omega   76.00  158.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   30.0000 -180.0000 164

 21 omega   29.00   69.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -30.0000 80

 22 omega   77.00  118.50   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000    0.0000 83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0376650000
_diffrn_orient_matrix_UB_12      -0.0585750000
_diffrn_orient_matrix_UB_13      -0.0840813000
_diffrn_orient_matrix_UB_21      -0.1043812000
_diffrn_orient_matrix_UB_22      0.0345862000
_diffrn_orient_matrix_UB_23      -0.0164477000
_diffrn_orient_matrix_UB_31      0.0786717000
_diffrn_orient_matrix_UB_32      0.0853469000
_diffrn_orient_matrix_UB_33      -0.0142209000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31085
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         73.474
_diffrn_reflns_theta_min         3.903
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.269
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.1613
_exptl_crystal_size_mid          0.0986
_exptl_crystal_size_min          0.0723
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.901
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         12849
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0574
_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^)+(0.1181P)^2^+1.5554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10283
_reflns_number_total             12849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01572g2.cif
_cod_data_source_block           ap
_cod_original_cell_volume        3305.17(10)
_cod_database_code               7124606
_chemical_oxdiff_formula         'C146 H158 N10 Ni4 P8 S2'
_reflns_odcompleteness_completeness 99.46
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 C73-C67 \\sim C73A-C67A
 with sigma of 0.02
 C73A-C72A \\sim C73A-C68A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C67) = Uanis(C67A) = Uanis(C68) = Uanis(C68A) = Uanis(C69) = Uanis(C69A)
= Uanis(C70) = Uanis(C70A) = Uanis(C71) = Uanis(C71A) = Uanis(C72) =
Uanis(C72A) = Uanis(C73) = Uanis(C73A)
4. Others
 Fixed Sof: C67A(0.21) C68A(0.21) H68A(0.21) C69A(0.21) H69A(0.21) C70A(0.21)
 H70A(0.21) C71A(0.21) H71A(0.21) C72A(0.21) H72A(0.21) C73A(0.21) H73A(0.21)
 H73B(0.21) H73C(0.21) C67(0.79) C68(0.79) H68(0.79) C69(0.79) H69(0.79)
 C70(0.79) H70(0.79) C71(0.79) H71(0.79) C72(0.79) H72(0.79) C73(0.79)
 H73D(0.79) H73E(0.79) H73F(0.79)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C26(H26), C28(H28), C35(H35), C37(H37), C44(H44),
 C46(H46), C53(H53), C55(H55), C68A(H68A), C69A(H69A), C70A(H70A), C71A(H71A),
 C72A(H72A), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72)
5.b Fitted hexagon refined as free rotating group:
 C67A(C68A,C69A,C70A,C71A,C72A), C67(C68,C69,C70,C71,C72)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C50(H50A,H50B,H50C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C73A(H73A,H73B,H73C), C66(H66A,H66B,H66C), C73(H73D,H73E,
 H73F)
;
_shelx_res_checksum              89600
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'