Steric control on the coordination behaviour of carbazole thiosemicarbazones towards [RuH(Cl)(CO)(AsPh3)3]: a combined experimental and theoretical study
Raj Kumar, Ramasamy; Ramesh, Rengan; Małecki, Jan Grzegorz; New J. Chem. 40 (2016) 10084–; doi:10.1039/C6NJ02430K

data_7055847
_publ_section_title
;
 Steric control on the coordination behaviour of carbazole
 thiosemicarbazones towards [RuH(Cl)(CO)(AsPh3)3]: a combined experimental
 and theoretical study
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              10084
_journal_paper_doi               10.1039/C6NJ02430K
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C59 H48 As2 N4 O Ru S, C2 H3 N'
_chemical_formula_sum            'C61 H51 As2 N5 O Ru S'
_chemical_formula_weight         1153.04
_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   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-01 deposited with the CCDC.
2016-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                86.508(4)
_cell_angle_beta                 71.243(5)
_cell_angle_gamma                67.212(5)
_cell_formula_units_Z            2
_cell_length_a                   12.3121(7)
_cell_length_b                   13.7064(7)
_cell_length_c                   17.7353(9)
_cell_measurement_reflns_used    6306
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.4310
_cell_measurement_theta_min      4.0480
_cell_volume                     2605.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w    -41.00  51.00   1.00   20.49    --  -11.78  69.00   8.00   92
  2  \w     48.00  74.00   1.00   20.49    --    9.90  38.00  90.00   26
  3  \w     22.00  48.00   1.00   20.49    --  -11.78  38.00-120.00   26
  4  \w    -82.00   9.00   1.00   20.49    --  -11.78 -57.00  90.00   91
  5  \w    -85.00   9.00   1.00   20.49    --  -11.78 -69.00-124.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0480168000
_diffrn_orient_matrix_UB_12      -0.0187736000
_diffrn_orient_matrix_UB_13      0.0177517000
_diffrn_orient_matrix_UB_21      -0.0299983000
_diffrn_orient_matrix_UB_22      0.0255407000
_diffrn_orient_matrix_UB_23      -0.0280439000
_diffrn_orient_matrix_UB_31      0.0340075000
_diffrn_orient_matrix_UB_32      -0.0465048000
_diffrn_orient_matrix_UB_33      -0.0263041000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23594
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.634
_diffrn_reflns_theta_min         3.370
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       plate
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.755
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         12414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0850P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8113
_reflns_number_total             12414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj02430k2.cif
_cod_data_source_block           rrk303c
_cod_depositor_comments
'Adding full bibliography for 7055846--7055847.cif.'
_cod_database_code               7055847
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Ru1 As2 N5 O1 C61 H51'
_reflns_odcompleteness_completeness 99.79
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
2.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C3(H3A), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15),
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27),
  C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44), C45(H45),
  C46(H46), C47(H47), C49(H49), C50(H50), C51(H51), C52(H52), C53(H53),
 C55(H55), C56(H56), C57(H57), C58(H58), C59(H59)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              21114
_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 1.304
_oxdiff_exptl_absorpt_empirical_full_min 0.780