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_7119343
_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 Se4 Zr2'
_chemical_formula_sum            'C52 H84 P2 Se4 Zr2'
_chemical_formula_weight         1269.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-02
_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                 102.8354(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.2831(3)
_cell_length_b                   9.91947(18)
_cell_length_c                   18.6250(3)
_cell_measurement_reflns_used    4734
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.2460
_cell_measurement_theta_min      3.3540
_cell_volume                     2753.00(9)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -66.00   22.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.0756   57.0000 -150.0000 176

  2 omega  -50.00   27.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.0756   38.0000  120.0000 154

  3 omega   38.00   86.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  150.0000 96

  4 omega   32.00   81.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 98

  5 omega   34.00  120.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000 -125.0000  120.0000 172

  6 omega   86.00  173.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000 -180.0000 174

  7 omega   41.00  127.00   0.5000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -77.0000 -120.0000 172

  8 omega   14.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       44.0756   77.0000  120.0000 174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0362753000
_diffrn_orient_matrix_UB_12      -0.1231329000
_diffrn_orient_matrix_UB_13      -0.0346516000
_diffrn_orient_matrix_UB_21      0.0436835000
_diffrn_orient_matrix_UB_22      0.0946879000
_diffrn_orient_matrix_UB_23      -0.0476232000
_diffrn_orient_matrix_UB_31      0.0863063000
_diffrn_orient_matrix_UB_32      0.0040374000
_diffrn_orient_matrix_UB_33      0.0610369000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10319
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.059
_diffrn_reflns_theta_max         67.059
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'Microfocus X-ray source'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.908
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.681
_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            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       plate
_exptl_crystal_F_000             1284
_exptl_crystal_preparation       -
_exptl_crystal_recrystallization_method -
_exptl_crystal_size_max          0.0857
_exptl_crystal_size_mid          0.0662
_exptl_crystal_size_min          0.0517
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0684P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4053
_reflns_number_total             4872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09427a2.cif
_cod_data_source_block           sean804_abs
_cod_depositor_comments
'Adding full bibliography for 7119342--7119344.cif.'
_cod_database_code               7119343
_chemical_oxdiff_formula         C26H42ZrPSe2
_reflns_odcompleteness_completeness 98.91
_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), C3(H3), C10(H10), C11(H11), C4(H4)
2.b Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C143(H14A,H14B,H14C), C61(H61A,H61B,H61C), C142(H14D,
 H14E,H14F), C133(H13A,H13B,H13C), C132(H13D,H13E,H13F), C131(H13G,H13H,H13I),
 C73(H73A,H73B,H73C), C71(H71A,H71B,H71C), C62(H62A,H62B,H62C), C141(H14G,H14H,
 H14I), C63(H63A,H63B,H63C)
;
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method -
_olex2_submission_special_instructions 'No special instructions were received'