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_7044409
_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         'C46 H42 Cl4 N4 O2 P2 Ru2 S2'
_chemical_formula_sum            'C46 H42 Cl4 N4 O2 P2 Ru2 S2'
_chemical_formula_weight         1152.83
_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     dual
_audit_creation_date             2017-03-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-03-25 deposited with the CCDC.
2017-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.263(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3765(2)
_cell_length_b                   9.48940(10)
_cell_length_c                   16.8296(3)
_cell_measurement_reflns_used    14431
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.9040
_cell_measurement_theta_min      5.3760
_cell_volume                     2357.41(6)
_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    '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 0.997
_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     24.00  61.00   1.00    1.00    --   37.66  57.00  30.00   37
  2  \w     65.00 103.00   1.00    1.00    --   37.66  38.00  30.00   38
  3  \w     80.00 105.00   1.00    1.00    --   37.66  57.00  30.00   25
  4  \w     68.00 104.00   1.00    1.00    --   37.66  38.00 -30.00   36
  5  \w     74.00 101.00   1.00    1.00    --   37.66  19.00 -90.00   27
  6  \w     61.00  94.00   1.00    1.00    --   37.66  77.00 -90.00   33
  7  \w     71.00  98.00   1.00    1.00    --   37.66  77.00-180.00   27
  8  \w     29.00  73.00   1.00    1.00    --   37.66  57.00-180.00   44
  9  \w     25.00  66.00   1.00    1.00    --   37.66  77.00-180.00   41
 10  \w     12.00  38.00   1.00    1.00    --   37.66  77.00 -90.00   26
 11  \w     15.00  74.00   1.00    1.00    --   37.66  77.00 -30.00   59
 12  \w     44.00  98.00   1.00    1.00    --   37.66  38.00   0.00   54
 13  \w     67.00 105.00   1.00    1.00    --   37.66  77.00  60.00   38
 14  \w     69.00  96.00   1.00    1.00    --   37.66  57.00 120.00   27
 15  \w     41.00  67.00   1.00    4.00    --  111.00 -12.00  30.00   26
 16  \w     49.00  74.00   1.00    4.00    --  111.00 -50.00   0.00   25
 17  \w     59.00  86.00   1.00    4.00    --  111.00 -52.00 -30.00   27
 18  \w     86.00 113.00   1.00    4.00    --  111.00 -77.00 -60.00   27
 19  \w     82.00 113.00   1.00    4.00    --  111.00-111.00   0.00   31
 20  \w     77.00 114.00   1.00    4.00    --  111.00-111.00 -60.00   37
 21  \w    120.00 145.00   1.00    4.00    --  111.00 -92.00-150.00   25
 22  \w     92.00 125.00   1.00    4.00    --  111.00 -25.00-180.00   33
 23  \w    128.00 178.00   1.00    4.00    --  111.00  25.00 -90.00   50
 24  \w    151.00 176.00   1.00    4.00    --  111.00  64.00 -30.00   25
 25  \w    140.00 177.00   1.00    4.00    --  111.00  64.00 -90.00   37
 26  \w    134.00 177.00   1.00    4.00    --  111.00 111.00 -60.00   43
 27  \w    129.00 156.00   1.00    4.00    --  111.00  64.00-150.00   27
 28  \w    118.00 145.00   1.00    4.00    --  111.00  25.00 -30.00   27
 29  \w    110.00 156.00   1.00    4.00    --  111.00 -12.00  30.00   46
 30  \w    137.00 165.00   1.00    4.00    --  111.00  38.00  60.00   28
 31  \w    122.00 149.00   1.00    4.00    --  111.00  77.00   0.00   27
 32  \w    103.00 130.00   1.00    4.00    --  111.00  25.00   0.00   27
 33  \w    100.00 169.00   1.00    4.00    --  111.00  38.00  30.00   69
 34  \w    103.00 170.00   1.00    4.00    --  111.00  38.00 150.00   67
 35  \w     92.00 119.00   1.00    4.00    --  111.00  77.00   0.00   27
 36  \w     98.00 123.00   1.00    4.00    --  111.00  38.00 -30.00   25
 37  \w     93.00 151.00   1.00    4.00    --  111.00  38.00 -90.00   58
 38  \w    100.00 134.00   1.00    4.00    --  111.00  50.00-120.00   34
 39  \w     95.00 124.00   1.00    4.00    --  111.00  64.00-150.00   29
 40  \w     63.00  90.00   1.00    4.00    --  111.00 -43.00-165.94   27
 41  \w     60.00 127.00   1.00    4.00    --  111.00 -64.00-180.00   67
 42  \w     76.00 103.00   1.00    4.00    --  111.00 -50.00 -90.00   27
 43  \w     60.00 127.00   1.00    4.00    --  111.00 -64.00 -90.00   67
 44  \w     56.00 114.00   1.00    4.00    --  111.00-111.00  60.00   58
 45  \w     89.00 122.00   1.00    4.00    --  111.00 -92.00 120.00   33
 46  \w     98.00 125.00   1.00    4.00    --  111.00 -77.00 120.00   27
 47  \w     87.00 116.00   1.00    4.00    --  111.00-111.00 150.00   29
 48  \w     75.00 114.00   1.00    4.00    --  111.00-111.00  90.00   39
 49  \w     87.00 121.00   1.00    4.00    --  111.00 -50.00  60.00   34
 50  \w     98.00 128.00   1.00    4.00    --  111.00  38.00  60.00   30
 51  \w     52.00 103.00   1.00    4.00    --  111.00 -50.00 150.00   51
 52  \w     51.00 108.00   1.00    4.00    --  111.00-111.00 120.00   57
 53  \w     50.00  78.00   1.00    4.00    --  111.00 -77.00 120.00   28
 54  \w     46.00  73.00   1.00    4.00    --  111.00 -92.00 120.00   27
 55  \w     43.00  68.00   1.00    4.00    --  111.00-111.00 150.00   25
 56  \w     54.00  81.00   1.00    4.00    --  111.00 -50.00  60.00   27
 57  \w     54.00  81.00   1.00    4.00    --  111.00 -64.00  30.00   27
 58  \w     41.00  69.00   1.00    4.00    --  111.00-111.00  30.00   28
 59  \w     52.00 111.00   1.00    4.00    --  111.00 -25.00   0.00   59
 60  \w     47.00  74.00   1.00    1.00    --   37.66 -99.00  60.00   27
 61  \w     50.00  77.00   1.00    1.00    --   37.66 -99.00 120.00   27
 62  \w     44.00  71.00   1.00    1.00    --   37.66-125.00 150.00   27
 63  \w     29.00  54.00   1.00    1.00    --   37.66 -57.00 150.00   25
 64  \w      4.00  37.00   1.00    1.00    --   37.66 -99.00 120.00   33
 65  \w      8.00  33.00   1.00    1.00    --   37.66 -99.00  60.00   25
 66  \w     16.00  43.00   1.00    1.00    --   37.66 -57.00  30.00   27
 67  \w     13.00  54.00   1.00    1.00    --   37.66 -77.00   0.00   41
 68  \w     42.00  86.00   1.00    1.00    --   37.66-125.00 -60.00   44
 69  \w     47.00  72.00   1.00    1.00    --   37.66 -99.00-150.00   25
 70  \w     32.00  64.00   1.00    1.00    --   37.66-125.00-180.00   32
 71  \w     33.00  59.00   1.00    1.00    --   37.66 -77.00 -90.00   26
 72  \w    -13.00  14.00   1.00    1.00    --   37.66 -57.00-120.00   27
 73  \w    -21.00   6.00   1.00    1.00    --   37.66 -77.00 -90.00   27
 74  \w    -26.00  13.00   1.00    1.00    --   37.66 -57.00-150.00   39
 75  \w     12.00  51.00   1.00    1.00    --   37.66  19.00 -90.00   39
 76  \w     22.00  65.00   1.00    1.00    --   37.66  38.00 -30.00   43
 77  \w     24.00  49.00   1.00    1.00    --   37.66  77.00  60.00   25
 78  \w     42.00  98.00   1.00    4.00    --  111.00 -38.00-120.00   56
 79  \w     63.00 108.00   1.00    4.00    --  111.00 -92.00-150.00   45
 80  \w    -27.00   0.00   1.00    1.00    --   37.66 -77.00   0.00   27
 81  \w    -29.00   7.00   1.00    1.00    --   37.66 -57.00 150.00   36
 82  \w     79.00 104.00   1.00    4.00    --  111.00 178.00-120.00   25
;
_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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0935763000
_diffrn_orient_matrix_UB_12      -0.0615848000
_diffrn_orient_matrix_UB_13      0.0448968000
_diffrn_orient_matrix_UB_21      -0.0458789000
_diffrn_orient_matrix_UB_22      -0.1129721000
_diffrn_orient_matrix_UB_23      0.0402473000
_diffrn_orient_matrix_UB_31      -0.0058108000
_diffrn_orient_matrix_UB_32      -0.0989385000
_diffrn_orient_matrix_UB_33      -0.0738700000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29400
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.790
_diffrn_reflns_theta_min         2.994
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.088
_exptl_absorpt_correction_T_max  0.52229
_exptl_absorpt_correction_T_min  0.48135
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       plate
_exptl_crystal_F_000             1160
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/EtOH'
_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.048
_exptl_crystal_size_rad          0.08
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0275
_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^)+(0.0375P)^2^+2.4273P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4345
_reflns_number_total             4750
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02420g2.cif
_cod_data_source_block           KMAb136_scale
_cod_database_code               7044409
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 98.60
_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: H11(0.034)
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46)
3.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C)
;
_shelx_res_checksum              69695
_ins_header
;
TITL KMAb136_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  15.376491   9.489351  16.829585  90.0000 106.2632  90.0000
ZERR    4.00   0.000239   0.000124   0.000264   0.0000   0.0017   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O P S Cl Ru
UNIT 92.00 84.00 8.00 4.00 4.00 4.00 8.00 4.00
TREF
HKLF 4
END
;
_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 1.884
_oxdiff_exptl_absorpt_empirical_full_min 0.716