Dihydrobis(methimazolyl)borato Complexes of Ruthenium and Osmium
Hill, Anthony; Foreman, Mark; Ma, Chenxi; Otten, Natalie E.; Sharma, Manab; Tshabang, Never; Ward, Jas S.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02420G

data_7044405
_publ_section_title
;
 Dihydrobis(methimazolyl)borato Complexes of Ruthenium and Osmium
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02420G
_journal_year                    2017
_chemical_formula_moiety         'C27 H28 B N4 O Os P S2, 2(C H Cl3)'
_chemical_formula_sum            'C29 H30 B Cl6 N4 O Os P S2'
_chemical_formula_weight         959.37
_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     dual
_audit_creation_date             2017-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2017-03-03 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                81.611(4)
_cell_angle_beta                 80.310(4)
_cell_angle_gamma                77.705(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5809(3)
_cell_length_b                   11.9170(5)
_cell_length_c                   16.4779(8)
_cell_measurement_reflns_used    12263
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1730
_cell_measurement_theta_min      3.7990
_cell_volume                     1800.13(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
  1 omega   37.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   57.0000   90.0000 66

  2 omega    0.00   27.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -77.0000 -120.0000 27

  3 omega   30.00   59.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -77.0000 -120.0000 29

  4 omega   23.00   89.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254 -125.0000   60.0000 66

  5 omega  -24.00  105.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254    0.0000 -120.0000 129

  6 omega   23.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   57.0000 -120.0000 78

  7 omega  -17.00   10.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -57.0000  -30.0000 27

  8 omega   -4.00   63.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -77.0000  120.0000 67

  9 omega   18.00   50.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -99.0000  -60.0000 32

 10 omega   58.00  100.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 42

 11 omega  112.00  175.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   90.0000 63

 12 omega   41.00   78.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -120.0000 37

 13 omega  101.00  138.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -60.0000 37

 14 omega   45.00   72.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 27

 15 omega   64.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 25

 16 omega   77.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -53.0000 -114.1116 27

 17 omega   95.00  155.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -150.0000 60

 18 omega   39.00   85.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 46

 19 omega  103.00  130.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -60.0000 27

 20 omega   51.00   95.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 44

 21 omega   43.00   96.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 53

 22 omega   71.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 44

 23 omega   74.00  100.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -120.0000 26

 24 omega   38.00   92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -22.0000 -178.9725 54

 25 omega   54.00  119.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -120.0000 65

 26 omega   62.00  116.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -120.0000 54

 27 omega   82.00  149.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 67

 28 omega   86.00  143.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 57

 29 omega  115.00  166.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 51

 30 omega   65.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000    0.0000 39

 31 omega   65.00  107.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 42

 32 omega   41.00   86.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 45

 33 omega   42.00  125.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   90.0000 83

 34 omega   77.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -30.0000 38

 35 omega  104.00  159.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 55

 36 omega   59.00  118.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  120.0000 59

 37 omega   83.00  141.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 58

 38 omega  104.00  130.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  150.0000 26

 39 omega   74.00   99.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 25

 40 omega   80.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -150.0000 28

 41 omega   69.00   94.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -42.0000  103.9474 25

 42 omega   62.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000   12.1812 29

 43 omega   80.00  106.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 26

 44 omega   54.00   81.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -20.0000  -72.3744 27

 45 omega  136.00  176.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -90.0000 40

 46 omega  121.00  169.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  120.0000 48

 47 omega   51.00   88.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -44.0000  -96.8803 37

 48 omega  141.00  166.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -120.0000 25

 49 omega   73.00  109.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -97.0000  167.7900 36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      -0.0301177000
_diffrn_orient_matrix_UB_12      0.0597673000
_diffrn_orient_matrix_UB_13      -0.0864230000
_diffrn_orient_matrix_UB_21      0.1613303000
_diffrn_orient_matrix_UB_22      -0.0341445000
_diffrn_orient_matrix_UB_23      -0.0337990000
_diffrn_orient_matrix_UB_31      -0.0265815000
_diffrn_orient_matrix_UB_32      -0.1140128000
_diffrn_orient_matrix_UB_33      -0.0224382000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19823
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.439
_diffrn_reflns_theta_min         3.821
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.546
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.1138
_exptl_crystal_size_mid          0.0374
_exptl_crystal_size_min          0.0251
_refine_diff_density_max         1.305
_refine_diff_density_min         -2.000
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         7083
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0512P)^2^+4.0559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6587
_reflns_number_total             7083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02420g2.cif
_cod_data_source_block           NEO-Os-Bm-H-1
_cod_database_code               7044405
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 96.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Others
 Fixed Uiso: H1(0.034)
3.a Ternary CH refined with riding coordinates:
 C101(H101), C201(H201)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C24(H24), C25(H25), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52),
  C53(H53), C54(H54), C55(H55), C56(H56)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              40251
_olex2_submission_special_instructions 'No special instructions were received'