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_7124605
_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, 2.5(C7 H8)'
_chemical_formula_sum            'C76.5 H83 N5 Ni2 P4 S'
_chemical_formula_weight         1345.83
_chemical_name_common            '[CpNi(IMes)]2(P4SCNPh)](tol)2.5'
_chemical_name_systematic        2a
_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                99.8667(19)
_cell_angle_beta                 99.819(2)
_cell_angle_gamma                98.0922(19)
_cell_formula_units_Z            2
_cell_length_a                   13.6251(4)
_cell_length_b                   14.0607(3)
_cell_length_c                   19.7007(5)
_cell_measurement_reflns_used    23012
_cell_measurement_temperature    122.8(7)
_cell_measurement_theta_max      66.5030
_cell_measurement_theta_min      4.2060
_cell_volume                     3607.33(17)
_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 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -28.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2837  -38.0000   30.0000 96

  2 omega   15.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2837   38.0000 -150.0000 97

  3 omega   -2.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2837 -125.0000  -30.0000 96

  4 omega   72.00  132.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  147.0671 60

  5 omega   91.00  130.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000 -142.5284 39

  6 omega   49.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   18.9323 30

  7 omega   48.00   84.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000 -142.5284 36

  8 omega   40.00   67.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000   95.6151 27

  9 omega   76.00  105.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000   95.6151 29

 10 omega   35.00  123.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  150.0000 88

 11 omega  135.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  150.0000 42

 12 omega   26.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   90.0000 37

 13 omega   57.00   94.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   90.0000 37

 14 omega   38.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -120.0000 28

 15 omega  143.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000   30.0000 25

 16 omega   11.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -150.0000 52

 17 omega   24.00   51.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000   30.0000 27

 18 omega   27.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -150.0000 50

 19 omega   99.00  124.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000 -150.0000 25

 20 omega   32.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  150.0000 65

 21 omega  112.00  152.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  150.0000 40

 22 omega   39.00   66.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -30.0000 27

 23 omega   21.00   54.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000   90.0000 33

 24 omega   14.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  -60.0000 62

 25 omega   66.00  141.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000   30.0000 75

 26 omega   11.00   64.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  120.0000 53

 27 omega   87.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   18.9323 35

 28 omega   39.00   90.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000   30.0000 51

 29 omega   77.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  -90.0000 27

 30 omega  136.00  163.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  -90.0000 27

 31 omega    8.00   43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -90.0000 -142.5284 35

 32 omega   74.00  163.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  -90.0000 89

 33 omega  113.00  166.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  125.0000  -60.0000 53

 34 omega   24.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000    0.0000 32

 35 omega   90.00  122.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -77.5590 32

 36 omega   70.00  124.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000   30.0000 54

 37 omega   29.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  -77.5590 49

 38 omega    8.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2837   77.0000  150.0000 112

 39 omega  -35.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2837  -38.0000  120.0000 103

 40 omega    8.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2837   77.0000  -30.0000 112

 41 omega    8.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2837   77.0000 -120.0000 112

 42 omega   12.00  115.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2837   57.0000   90.0000 103

 43 omega   60.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  150.0000 112

 44 omega   60.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -30.0000 112

 45 omega   66.00  168.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000 -120.0000 102

 46 omega   60.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -180.0000 112

 47 omega   60.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   90.0000 112

 48 omega   60.00  172.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000   30.0000 112

 49 omega   60.00  101.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000 -120.0000 41

 50 omega   63.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   61.0000  -60.0000 33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0018316000
_diffrn_orient_matrix_UB_12      -0.1043146000
_diffrn_orient_matrix_UB_13      -0.0406382000
_diffrn_orient_matrix_UB_21      -0.0820905000
_diffrn_orient_matrix_UB_22      0.0151485000
_diffrn_orient_matrix_UB_23      -0.0594366000
_diffrn_orient_matrix_UB_31      0.0827140000
_diffrn_orient_matrix_UB_32      0.0405949000
_diffrn_orient_matrix_UB_33      -0.0371097000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            65571
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.623
_diffrn_reflns_theta_min         3.672
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.096
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.713
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             1418
_exptl_crystal_size_max          0.2672
_exptl_crystal_size_mid          0.1865
_exptl_crystal_size_min          0.1779
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         12645
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1251P)^2^+7.6586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2095
_refine_ls_wR_factor_ref         0.2185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10852
_reflns_number_total             12645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01572g2.cif
_cod_data_source_block           ap
_cod_original_cell_volume        3607.32(16)
_cod_original_formula_sum        'C76.50 H83 N5 Ni2 P4 S'
_cod_database_code               7124605
_chemical_oxdiff_formula         'C153 H164 N10 Ni4 P8 S2'
_reflns_odcompleteness_completeness 97.99
_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
 C69-C74 \\sim C73-C74
 with sigma of 0.02
 C74-C68 \\sim C74A-C68A
 with sigma of 0.02
 C69A-C74A \\sim C73A-C74A
 with sigma of 0.02
 C76-C81 \\sim C78-C81
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(C74) = Uiso(C74A)
Uiso(C68) = Uiso(C68A)
Uiso(C69) = Uiso(C69A)
Uiso(C70) = Uiso(C70A)
Uiso(C71) = Uiso(C71A)
Uiso(C72) = Uiso(C72A)
Uiso(C73) = Uiso(C73A)
Uiso(C75) = Uiso(C76) = Uiso(C77) = Uiso(C78) = Uiso(C79) = Uiso(C80) =
Uiso(C81)
4. Others
 Fixed Sof: C68(0.75) C69(0.75) H69(0.75) C70(0.75) H70(0.75) C71(0.75)
 H71(0.75) C72(0.75) H72(0.75) C73(0.75) H73(0.75) C74(0.75) H74A(0.75)
 H74B(0.75) H74C(0.75) C74A(0.25) H74D(0.25) H74E(0.25) H74F(0.25) C68A(0.25)
 C69A(0.25) H69A(0.25) C70A(0.25) H70A(0.25) C71A(0.25) H71A(0.25) C72A(0.25)
 H72A(0.25) C73A(0.25) H73A(0.25) C75(0.5) H75(0.5) C76(0.5) H76(0.5) C77(0.5)
 C78(0.5) H78(0.5) C80(0.5) H80(0.5) C79(0.5) H79(0.5) C81(0.5) H81A(0.5)
 H81B(0.5) H81C(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C41(H41), C15(H15), C5(H5), C13(H13), C14(H14), C4(H4), C6(H6), C32(H32),
 C3(H3), C7(H7), C39(H39), C11(H11), C21(H21), C12(H12), C16(H16), C17(H17),
 C30(H30), C9(H9), C8(H8), C23(H23), C48(H48), C50(H50), C56(H56), C57(H57),
 C60(H60), C58(H58), C62(H62), C64(H64), C66(H66), C65(H65), C59(H59), C63(H63),
  C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C69A(H69A), C70A(H70A),
 C71A(H71A), C72A(H72A), C73A(H73A), C75(H75), C76(H76), C78(H78), C80(H80),
 C79(H79)
5.b Fitted hexagon refined as free rotating group:
 C68(C69,C70,C71,C72,C73), C68A(C69A,C70A,C71A,C72A,C73A), C75(C76,C77,C78,C80,
 C79)
5.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C43(H43A,H43B,H43C), C34(H34A,H34B,H34C), C36(H36A,H36B,
 H36C), C25(H25A,H25B,H25C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C), C44(H44A,
 H44B,H44C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C26(H26A,H26B,H26C),
 C53(H53A,H53B,H53C), C67(H67A,H67B,H67C), C74(H74A,H74B,H74C), C74A(H74D,H74E,
 H74F), C81(H81A,H81B,H81C)
;
_shelx_res_checksum              33502
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'