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_7119344
_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 As2 S4 Zr2, 4(C7 H8)'
_chemical_formula_sum            'C80 H116 As2 S4 Zr2'
_chemical_formula_weight         1538.24
_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
_audit_creation_date             2016-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2016-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3864(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.6043(2)
_cell_length_b                   12.6538(2)
_cell_length_c                   24.3651(4)
_cell_measurement_reflns_used    7550
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.1590
_cell_measurement_theta_min      3.5670
_cell_volume                     3868.89(11)
_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
;
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 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega -113.00  -20.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.0756  -57.0000  -60.0000 93

  2 omega -132.00  -35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -44.0756 -178.0000  -60.0000 97

  3 omega   32.00   91.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   60.0000 59

  4 omega   58.00   91.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  150.0000 33

  5 omega   33.00   91.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  120.0000 58

  6 omega   33.00  105.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000    0.0000 72

  7 omega   84.00  165.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000 -150.0000 81

  8 omega   23.00  105.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -60.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0290740000
_diffrn_orient_matrix_UB_12      0.1182937000
_diffrn_orient_matrix_UB_13      0.0020747000
_diffrn_orient_matrix_UB_21      0.1053420000
_diffrn_orient_matrix_UB_22      -0.0258122000
_diffrn_orient_matrix_UB_23      0.0347456000
_diffrn_orient_matrix_UB_31      0.0560813000
_diffrn_orient_matrix_UB_32      -0.0123210000
_diffrn_orient_matrix_UB_33      -0.0531180000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13931
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.034
_diffrn_reflns_theta_max         67.034
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'Microfocus X-ray source'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.463
_exptl_absorpt_correction_T_max  0.826
_exptl_absorpt_correction_T_min  0.717
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.1288
_exptl_crystal_size_mid          0.0947
_exptl_crystal_size_min          0.0554
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.073
_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     411
_refine_ls_number_reflns         6855
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0399P)^2^+2.0824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5754
_reflns_number_total             6855
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09427a2.cif
_cod_data_source_block           sean277_2_1_abscorr
_cod_depositor_comments
'Adding full bibliography for 7119342--7119344.cif.'
_cod_database_code               7119344
_chemical_oxdiff_formula         C40H58ZrAsS2
_chemical_oxdiff_usercomment     'purple block'
_reflns_odcompleteness_completeness 99.12
_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:
 C3(H3), C11(H11), C1(H1), C4(H4), C8(H8), C10(H10), C26(H26), C22(H22),
 C25(H25), C23(H23), C24(H24), C16(H16), C17(H17), C18(H18), C19(H19), C15(H15)
2.b Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C131(H13A,H13B,H13C), C132(H13D,H13E,H13F), C63(H63A,
 H63B,H63C), C141(H14A,H14B,H14C), C73(H73A,H73B,H73C), C133(H13G,H13H,H13I),
 C61(H61A,H61B,H61C), C71(H71A,H71B,H71C), C62(H62A,H62B,H62C), C143(H14D,H14E,
 H14F), C142(H14G,H14H,H14I), C28(H28A,H28B,H28C), C21(H21A,H21B,H21C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'