Transformation of nortricyclane type cage compounds P4S3, P4Se3 and As4S3 by [Cp''2Zr(CO)2].
Seitz, A. E.; Heinl, V.; Timoshkin, A. Y.; Scheer, M.; Chemical communications (Cambridge, England) 53 (2017) 1172–1175; doi:10.1039/c6cc09427a

data_7119342
_publ_section_title
;
 Transformation of nortricyclane type cage compounds P4S3, P4Se3 and As4S3
 by [Cp''2Zr(CO)2].
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1172
_journal_page_last               1175
_journal_paper_doi               10.1039/c6cc09427a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C52 H84 P2 S4 Zr2'
_chemical_formula_sum            'C52 H84 P2 S4 Zr2'
_chemical_formula_weight         1081.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2016-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8930(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.7202(5)
_cell_length_b                   13.6790(2)
_cell_length_c                   16.2972(3)
_cell_measurement_reflns_used    9074
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.3020
_cell_measurement_theta_min      3.5510
_cell_volume                     5481.74(17)
_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, 2008)'
_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 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega -104.00   -9.00   0.5000    0.5000
omega____ theta____ kappa____ phi______ frames
    -      -44.3256  136.0000    6.0000 190

  2 omega  -50.00   26.00   0.5000    0.5000
omega____ theta____ kappa____ phi______ frames
    -      -44.3256   38.0000 -150.0000 152

  3 omega   33.00  135.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000  120.0000 204

  4 omega   32.00   91.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  150.0000 118

  5 omega   81.00  177.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000 -180.0000 192

  6 omega   82.00  173.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000   90.0000 182

  7 omega   33.00  121.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000   90.0000 176

  8 omega   20.00  114.00   0.5000    0.5000
omega____ theta____ kappa____ phi______ frames
    -       44.3256   57.0000   60.0000 188

  9 omega   14.00  116.00   0.5000    0.5000
omega____ theta____ kappa____ phi______ frames
    -       44.3256   77.0000  -90.0000 204

 10 omega   68.00  125.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   15.0000  -30.0000 114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0565958000
_diffrn_orient_matrix_UB_12      -0.0209094000
_diffrn_orient_matrix_UB_13      -0.0276399000
_diffrn_orient_matrix_UB_21      -0.0268361000
_diffrn_orient_matrix_UB_22      -0.0434268000
_diffrn_orient_matrix_UB_23      -0.0814288000
_diffrn_orient_matrix_UB_31      0.0002428000
_diffrn_orient_matrix_UB_32      0.1017996000
_diffrn_orient_matrix_UB_33      -0.0404307000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14672
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.071
_diffrn_reflns_theta_max         67.071
_diffrn_reflns_theta_min         3.595
_diffrn_source                   'Microfocus X-ray source'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.325
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.511
_exptl_absorpt_correction_type   gaussian
_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)
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 bluish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       plate
_exptl_crystal_F_000             2280
_exptl_crystal_recrystallization_method 'crystalized out of n-hexane'
_exptl_crystal_size_max          0.2127
_exptl_crystal_size_mid          0.1206
_exptl_crystal_size_min          0.0323
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0526P)^2^+2.1550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4320
_reflns_number_total             4884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09427a2.cif
_cod_data_source_block           sean157_mc_abs
_cod_depositor_comments
'Adding full bibliography for 7119342--7119344.cif.'
_cod_original_cell_volume        5481.75(17)
_cod_database_code               7119342
_chemical_oxdiff_formula         C26H42ZrPS2
_reflns_odcompleteness_completeness 99.69
_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.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C1(H1), C10(H10), C3(H3), C4(H4), C11(H11)
2.b Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C71(H71A,H71B,H71C), C62(H62A,H62B,
 H62C), C133(H13A,H13B,H13C), C63(H63A,H63B,H63C), C61(H61A,H61B,H61C),
 C142(H14A,H14B,H14C), C143(H14D,H14E,H14F), C132(H13D,H13E,H13F), C131(H13G,
 H13H,H13I), C141(H14G,H14H,H14I)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id SeAn157
_olex2_submission_special_instructions 'No special instructions were received'