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_7044408
_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         'C33 H31 B2 N4 O3 P Ru S2, C H2 Cl2'
_chemical_formula_sum            'C34 H33 B2 Cl2 N4 O3 P Ru S2'
_chemical_formula_weight         834.32
_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                76.821(4)
_cell_angle_beta                 83.043(4)
_cell_angle_gamma                72.153(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1930(5)
_cell_length_b                   12.0791(5)
_cell_length_c                   14.4768(7)
_cell_measurement_reflns_used    11603
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.1840
_cell_measurement_theta_min      3.1410
_cell_volume                     1811.25(15)
_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 0.993
_diffrn_measurement_details
;
  1 omega   40.00   86.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254 -125.0000   60.0000 46

  2 omega   22.00   56.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   57.0000  -30.0000 34

  3 omega    1.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -57.0000 -180.0000 46

  4 omega   17.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -99.0000  150.0000 50

  5 omega  -31.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -57.0000  -30.0000 78

  6 omega   58.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   19.0000 -150.0000 33

  7 omega   61.00   87.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   57.0000  -30.0000 26

  8 omega    7.00   52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254   19.0000 -150.0000 45

  9 omega  -21.00   38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -57.0000   60.0000 59

 10 omega   50.00   83.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254 -125.0000  -90.0000 33

 11 omega  -35.00   64.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       36.0254  -19.0000 -180.0000 99

 12 omega   70.00  106.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   60.0000 36

 13 omega   70.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 29

 14 omega   60.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  150.0000 37

 15 omega   75.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 39

 16 omega   64.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 26

 17 omega   40.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000  150.0000 42

 18 omega   38.00  101.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -21.0000   99.0907 63

 19 omega   39.00   65.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 26

 20 omega   51.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 26

 21 omega   81.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000    0.0000 27

 22 omega   48.00   79.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 31

 23 omega   69.00  103.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    5.0000  -84.9206 34

 24 omega   86.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 29

 25 omega   88.00  145.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  150.0000 57

 26 omega   49.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000    0.0000 27

 27 omega  129.00  177.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   30.0000 48

 28 omega   40.00   66.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   30.0000 26

 29 omega   82.00  108.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -95.0000   30.0000 26

 30 omega   41.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 30

 31 omega   47.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 51

 32 omega  116.00  175.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   90.0000 59

 33 omega   51.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 26

 34 omega   79.00  123.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -90.0000 44

 35 omega   95.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 27

 36 omega   63.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000   30.0000 26

 37 omega  123.00  164.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 41

 38 omega   41.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 52

 39 omega   91.00  142.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 51

 40 omega   77.00  115.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 38

 41 omega   45.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 38

 42 omega   54.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 68

 43 omega   66.00  118.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000   30.0000 52

 44 omega  137.00  163.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 26

 45 omega   67.00  114.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -90.0000 47

 46 omega   56.00   82.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 26

 47 omega   40.00   84.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -34.0000  156.0762 44

 48 omega  119.00  167.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    5.0000  -84.9206 48

 49 omega  106.00  158.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -30.0000 52

 50 omega   75.00  101.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  150.0000 26

 51 omega   64.00  112.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -102.0000  -61.7027 48
;
_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      0.0203005000
_diffrn_orient_matrix_UB_12      0.0153063000
_diffrn_orient_matrix_UB_13      -0.1088095000
_diffrn_orient_matrix_UB_21      0.0518888000
_diffrn_orient_matrix_UB_22      0.1053139000
_diffrn_orient_matrix_UB_23      -0.0036263000
_diffrn_orient_matrix_UB_31      0.1336686000
_diffrn_orient_matrix_UB_32      -0.0859713000
_diffrn_orient_matrix_UB_33      0.0113746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18958
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.420
_diffrn_reflns_theta_min         3.926
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.688
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90997
_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    1.530
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.1879
_exptl_crystal_size_mid          0.0820
_exptl_crystal_size_min          0.0185
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7109
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0484P)^2^+0.7427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0792
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6679
_reflns_number_total             7109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02420g2.cif
_cod_data_source_block           ner26
_cod_database_code               7044408
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 96.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C24(H24), C25(H25), 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), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
2.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              46758
_olex2_submission_special_instructions 'No special instructions were received'