Experimental and computational preference for phosphine regioselectivity and stereoselective tripodal rotation in HOs3(CO)8(PPh3)2(μ-1,2-N,C-η1,κ1-C7H4NS)
Begum, Shahin A.; Chowdhury, Md. Arshad H.; Ghosh, Shishir; Tocher, Derek A.; Richmond, Michael G.; Yang, Li; Hardcastle, K. I.; Rosenberg, Edward; Kabir, Shariff E.; RSC Advances 8 (2018) 32672–; doi:10.1039/C8RA07400C

data_7231552
_publ_section_title
;
 Experimental and computational preference for phosphine regioselectivity
 and stereoselective tripodal rotation in
 HOs3(CO)8(PPh3)2(\m-1,2-N,C-\h1,\k1-C7H4NS)
;
_journal_issue                   57
_journal_name_full               'RSC Advances'
_journal_page_first              32672
_journal_paper_doi               10.1039/C8RA07400C
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C51 H35 N O8 Os3 P2 S'
_chemical_formula_sum            'C51 H35 N O8 Os3 P2 S'
_chemical_formula_weight         1454.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-28 deposited with the CCDC.
2018-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.376(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8799(6)
_cell_length_b                   15.0410(3)
_cell_length_c                   18.7314(5)
_cell_measurement_reflns_used    37509
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.3890
_cell_measurement_theta_min      4.1430
_cell_volume                     4723.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -31.00  36.00   1.00    5.49    --   11.17 -38.00  30.00   67
  2  \w    -12.00  84.00   1.00    5.49    --   11.17  38.00  90.00   96
  3  \w    -17.00  80.00   1.00    5.49    --   11.17  77.00 -30.00   97
  4  \w      7.00  84.00   1.00    5.49    --   11.17  38.00-120.00   77
  5  \w    -12.00  78.00   1.00    5.49    --   11.17  38.00-180.00   90
  6  \w      1.00  67.00   1.00    5.49    --   11.17-124.00 -86.03   66
  7  \w    -20.00  52.00   1.00    5.49    --   11.17 -99.00 150.00   72
  8  \w      6.00  70.00   1.00    5.49    --   11.17-129.00  26.92   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0046941000
_diffrn_orient_matrix_UB_12      -0.0373576000
_diffrn_orient_matrix_UB_13      -0.0205380000
_diffrn_orient_matrix_UB_21      -0.0411543000
_diffrn_orient_matrix_UB_22      -0.0099354000
_diffrn_orient_matrix_UB_23      -0.0153184000
_diffrn_orient_matrix_UB_31      -0.0086689000
_diffrn_orient_matrix_UB_32      0.0269886000
_diffrn_orient_matrix_UB_33      -0.0340809000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            74577
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.418
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.218
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.602
_refine_diff_density_min         -1.895
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         9274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0223P)^2^+17.8448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8472
_reflns_number_total             9274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra07400c1.cif
_cod_data_source_block           xstr0844
_cod_database_code               7231552
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Os3 P2 S1 N1 O7 C50 H35'
_chemical_oxdiff_usercomment     'SEK 41b'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29),
  C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37),
 C38(H38), C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47),
  C48(H48), C49(H49), C50(H50), C51(H51)
;
_olex2_date_sample_data_collection 2018-03-27
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id 'XSTR0844 : SEK 41b'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.548
_oxdiff_exptl_absorpt_empirical_full_min 0.690