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_7231553
_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         '2(C34 H20 N O9 Os3 P S), C H2 Cl2, O'
_chemical_formula_sum            'C69 H42 Cl2 N2 O19 Os6 P2 S2'
_chemical_formula_weight         2541.20
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-18
_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                100.9456(19)
_cell_angle_beta                 92.7106(19)
_cell_angle_gamma                90.9327(17)
_cell_formula_units_Z            2
_cell_length_a                   11.0561(2)
_cell_length_b                   16.0438(3)
_cell_length_c                   21.7248(5)
_cell_measurement_reflns_used    32792
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      29.2840
_cell_measurement_theta_min      3.1780
_cell_volume                     3777.99(13)
_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    '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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   32.00   70.00   1.0000   17.6300
omega____ theta____ kappa____ phi______ frames
    -       11.0092 -129.0000  122.1218 38

  2 omega  -11.00   78.00   1.0000   17.6300
omega____ theta____ kappa____ phi______ frames
    -       11.0092   38.0000  -90.0000 89

  3 omega  -17.00   69.00   1.0000   17.6300
omega____ theta____ kappa____ phi______ frames
    -       11.0092   77.0000    0.0000 86

  4 omega  -13.00   84.00   1.0000   17.6300
omega____ theta____ kappa____ phi______ frames
    -       11.0092   38.0000  150.0000 97

  5 omega  -59.00   34.00   1.0000   17.6300
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -38.0000   90.0000 93

  6 omega  -50.00   36.00   1.0000   17.6300
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -38.0000  -30.0000 86

  7 omega  -46.00   44.00   1.0000   17.6300
omega____ theta____ kappa____ phi______ frames
    -       11.0092  -77.0000 -150.0000 90

  8 omega   16.00   86.00   1.0000   17.6300
omega____ theta____ kappa____ phi______ frames
    -       11.0092 -153.0000  -16.2167 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0312971000
_diffrn_orient_matrix_UB_12      0.0042281000
_diffrn_orient_matrix_UB_13      0.0297358000
_diffrn_orient_matrix_UB_21      -0.0479593000
_diffrn_orient_matrix_UB_22      0.0241515000
_diffrn_orient_matrix_UB_23      0.0141890000
_diffrn_orient_matrix_UB_31      -0.0291240000
_diffrn_orient_matrix_UB_32      -0.0377866000
_diffrn_orient_matrix_UB_33      0.0048192000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61319
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.748
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29598
_exptl_absorpt_correction_type   multi-scan
_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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             2348
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.791
_refine_diff_density_min         -1.516
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         14819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0234
_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^)+(0.0221P)^2^+7.2541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0569
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13383
_reflns_number_total             14819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra07400c1.cif
_cod_data_source_block           xstr0374
_cod_original_cell_volume        3777.98(15)
_cod_database_code               7231553
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Os3 P1 S1 N1 O9 C34 H20'
_chemical_oxdiff_usercomment     AH156B
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: O22(0.5) O21(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C69(H69A,H69B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20),
 C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30),
  C31(H31), C32(H32), C33(H33), C34(H34), C46(H46), C47(H47), C48(H48),
 C49(H49), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59),
  C60(H60), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
;
_olex2_date_sample_data_collection 2015-02-18
_olex2_exptl_crystal_mounting_method 'Nylon Loop'
_olex2_submission_original_sample_id xstr0374
_olex2_submission_special_instructions 'No special instructions were received'