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_7124604
_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         'C52 H58 N4 Ni2 P4, 1.5(C7 H8)'
_chemical_formula_sum            'C62.5 H70 N4 Ni2 P4'
_chemical_formula_weight         1118.52
_chemical_name_common            {[CpNi(IMes)]2P4}1.5(tol)
_chemical_name_systematic        1
_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                79.4323(17)
_cell_angle_beta                 76.229(2)
_cell_angle_gamma                84.6926(19)
_cell_formula_units_Z            2
_cell_length_a                   12.4093(4)
_cell_length_b                   13.1987(2)
_cell_length_c                   18.3557(4)
_cell_measurement_reflns_used    14037
_cell_measurement_temperature    122.9(2)
_cell_measurement_theta_max      66.5330
_cell_measurement_theta_min      4.5510
_cell_volume                     2866.71(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   16.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337   57.0000  -90.0000 93

  2 omega   77.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -60.0000 33

  3 omega  124.00  150.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -60.0000 26

  4 omega  116.00  142.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000  -90.0000 26

  5 omega  133.00  171.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -60.0000 38

  6 omega  117.00  174.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000   30.0000 57

  7 omega   96.00  122.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000   42.8955 26

  8 omega   84.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -59.0000   25.6158 34

  9 omega   66.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   30.0000  -90.0000 29

 10 omega   64.00  114.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   77.0000  -60.0000 50

 11 omega   32.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000   30.0000 54

 12 omega   31.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000  -60.0000 46

 13 omega   96.00  122.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -105.4465 26

 14 omega   83.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -88.0000 -156.5212 48

 15 omega   47.00  131.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000   -5.3422 84

 16 omega   41.00   79.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000 -105.4465 38

 17 omega   19.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -59.0000   25.6158 44

 18 omega   42.00   68.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -91.0000   42.8955 26

 19 omega   33.00   81.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   30.0000 48

 20 omega   20.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000  120.0000 68

 21 omega   20.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   60.0000 47

 22 omega   14.00  107.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -93.0000  165.0458 93

 23 omega   -3.00   71.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337 -125.0000   60.0000 74

 24 omega   11.00   51.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  -60.0000 40

 25 omega   18.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -150.0000 49

 26 omega   10.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -88.0000 -156.5212 67

 27 omega  -30.00   71.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5337  -57.0000  120.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1099759000
_diffrn_orient_matrix_UB_12      0.0210574000
_diffrn_orient_matrix_UB_13      0.0182285000
_diffrn_orient_matrix_UB_21      0.0604605000
_diffrn_orient_matrix_UB_22      -0.0025884000
_diffrn_orient_matrix_UB_23      -0.0833612000
_diffrn_orient_matrix_UB_31      -0.0251129000
_diffrn_orient_matrix_UB_32      0.1169819000
_diffrn_orient_matrix_UB_33      -0.0199890000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25046
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.727
_diffrn_reflns_theta_min         4.565
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.674
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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 red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             1178
_exptl_crystal_size_max          0.3321
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.1681
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0498P)^2^+2.5553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9059
_reflns_number_total             10078
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01572g2.cif
_cod_data_source_block           ap
_cod_original_formula_sum        'C62.50 H70 N4 Ni2 P4'
_cod_database_code               7124604
_chemical_oxdiff_formula         'C125 H140 N8 Ni4 P8'
_reflns_odcompleteness_completeness 98.38
_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. Others
 Fixed Sof: C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C1H(0.5) H1H(0.5) C1C(0.5)
 C1D(0.5) H1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5) C1G(0.5) H1G(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C32(H32), C30(H30), C31(H31), C20(H20), C33(H33), C34(H34), C2(H2), C13(H13),
 C39(H39), C22(H22), C11(H11), C3(H3), C29(H29), C28(H28), C6(H6), C5(H5),
 C48(H48), C46(H46), C7(H7), C4(H4), C37(H37), C8(H8), C1H(H1H), C1D(H1D),
 C1E(H1E), C1F(H1F), C1G(H1G), C1I(H1I), C1J(H1J), C1K(H1K), C1L(H1L), C1M(H1M)
3.b Fitted hexagon refined as free rotating group:
 C1H(C1C,C1D,C1E,C1F,C1G)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C43(H43A,H43B,H43C), C52(H52A,H52B,H52C), C17(H17A,H17B,
 H17C), C24(H24A,H24B,H24C), C50(H50A,H50B,H50C), C15(H15A,H15B,H15C), C25(H25A,
 H25B,H25C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C16(H16A,H16B,H16C),
 C51(H51A,H51B,H51C), C1B(H1BA,H1BB,H1BC), C1N(H1NA,H1NB,H1NC)
;
_shelx_res_checksum              43280
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'