Methimazolyl based diptych bicyclo-[3.3.0]-ruthenaboratranes.
Ma, Chenxi; Hill, Anthony F.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1976–1992; doi:10.1039/c8dt04813d

data_7048494
_publ_section_title
;
 Methimazolyl based diptych bicyclo-[3.3.0]-ruthenaboratranes.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1976
_journal_page_last               1992
_journal_paper_doi               10.1039/c8dt04813d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C35 H32 B N4 O P Ru S2, C H Cl3'
_chemical_formula_sum            'C36 H33 B Cl3 N4 O P Ru S2'
_chemical_formula_weight         850.98
_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             2018-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-26 deposited with the CCDC.
2019-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                73.725(4)
_cell_angle_beta                 82.147(4)
_cell_angle_gamma                65.670(6)
_cell_formula_units_Z            2
_cell_length_a                   9.9810(7)
_cell_length_b                   11.0018(6)
_cell_length_c                   19.3279(8)
_cell_measurement_reflns_used    10533
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.4880
_cell_measurement_theta_min      4.8480
_cell_volume                     1855.8(2)
_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 0.993
_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      9.00  87.00   1.00    2.00    --   36.95  19.00  60.00   78
  2  \w     60.00  99.00   1.00    2.00    --   36.95  57.00  60.00   39
  3  \w     49.00 104.00   1.00    2.00    --   36.95  57.00 -60.00   55
  4  \w     92.00 126.00   1.00    5.00    --  111.00 -50.00 -90.00   34
  5  \w    100.00 128.00   1.00    5.00    --  111.00 -38.00-120.00   28
  6  \w     94.00 136.00   1.00    5.00    --  111.00 -77.00-120.00   42
  7  \w     87.00 120.00   1.00    5.00    --  111.00-124.00-115.00   33
  8  \w     82.00 114.00   1.00    5.00    --  111.00-111.00-120.00   32
  9  \w     70.00  98.00   1.00    5.00    --  111.00-111.00 -30.00   28
 10  \w     99.00 124.00   1.00    5.00    --  111.00 -77.00   0.00   25
 11  \w     99.00 124.00   1.00    5.00    --  111.00 -64.00   0.00   25
 12  \w    104.00 129.00   1.00    5.00    --  111.00 -38.00  60.00   25
 13  \w     87.00 114.00   1.00    5.00    --  111.00 -92.00  90.00   27
 14  \w    103.00 128.00   1.00    5.00    --  111.00 -50.00 150.00   25
 15  \w     81.00 115.00   1.00    5.00    --  111.00-111.00 150.00   34
 16  \w     78.00 105.00   1.00    5.00    --  111.00 -64.00 120.00   27
 17  \w     81.00 114.00   1.00    5.00    --  111.00 -28.00  44.36   33
 18  \w    107.00 133.00   1.00    5.00    --  111.00  25.00 -30.00   26
 19  \w    100.00 172.00   1.00    5.00    --  111.00  38.00   0.00   72
 20  \w    133.00 169.00   1.00    5.00    --  111.00  50.00  60.00   36
 21  \w    145.00 176.00   1.00    5.00    --  111.00  38.00 120.00   31
 22  \w    105.00 177.00   1.00    5.00    --  111.00 111.00   0.00   72
 23  \w    113.00 147.00   1.00    5.00    --  111.00  64.00-120.00   34
 24  \w    136.00 178.00   1.00    5.00    --  111.00  64.00-150.00   42
 25  \w    129.00 178.00   1.00    5.00    --  111.00  25.00-180.00   49
 26  \w    111.00 136.00   1.00    5.00    --  111.00  50.00-180.00   25
 27  \w    102.00 128.00   1.00    5.00    --  111.00  64.00-150.00   26
 28  \w     86.00 164.00   1.00    5.00    --  111.00  25.00 -90.00   78
 29  \w     85.00 117.00   1.00    5.00    --  111.00  77.00  30.00   32
 30  \w     95.00 139.00   1.00    5.00    --  111.00  38.00 120.00   44
 31  \w     58.00 100.00   1.00    5.00    --  111.00 -77.00 120.00   42
 32  \w     63.00  89.00   1.00    5.00    --  111.00-111.00  90.00   26
 33  \w     42.00 115.00   1.00    5.00    --  111.00-111.00  60.00   73
 34  \w     62.00 107.00   1.00    5.00    --  111.00 -92.00 -30.00   45
 35  \w     70.00 114.00   1.00    5.00    --  111.00-111.00 -60.00   44
 36  \w     49.00  75.00   1.00    5.00    --  111.00 -38.00  60.00   26
 37  \w     56.00 104.00   1.00    5.00    --  111.00 -16.00  59.41   48
 38  \w     52.00 115.00   1.00    5.00    --  111.00 -50.00  60.00   63
 39  \w     42.00  68.00   1.00    5.00    --  111.00-111.00   0.00   26
 40  \w     51.00  77.00   1.00    5.00    --  111.00-111.00 -90.00   26
 41  \w     45.00  70.00   1.00    5.00    --  111.00-111.00-150.00   25
 42  \w     44.00 128.00   1.00    5.00    --  111.00 -50.00-150.00   84
 43  \w     43.00  75.00   1.00    5.00    --  111.00 -38.00-120.00   32
 44  \w     39.00  85.00   1.00    2.00    --   36.95-125.00-180.00   46
 45  \w     24.00  76.00   1.00    2.00    --   36.95 -99.00 -90.00   52
 46  \w     29.00  82.00   1.00    2.00    --   36.95-125.00  60.00   53
 47  \w     26.00  51.00   1.00    2.00    --   36.95 -57.00 150.00   25
 48  \w     16.00  43.00   1.00    2.00    --   36.95 -38.00 120.00   27
 49  \w     20.00  61.00   1.00    2.00    --   36.95  38.00 150.00   41
 50  \w     54.00  90.00   1.00    5.00    --  111.00 -50.00 150.00   36
 51  \w     43.00  71.00   1.00    5.00    --  111.00 -92.00  90.00   28
 52  \w    -31.00  -3.00   1.00    2.00    --   36.95 -38.00 120.00   28
 53  \w    -30.00  10.00   1.00    2.00    --   36.95 -57.00 150.00   40
 54  \w   -101.00 -62.00   1.00    2.00    --  -36.95-148.00  80.00   39
 55  \w     23.00  86.00   1.00    2.00    --   36.95  57.00 -90.00   63
 56  \w     67.00  93.00   1.00    5.00    --  111.00 178.00-150.00   26
 57  \w    105.00 130.00   1.00    5.00    --  111.00 178.00-150.00   25
 58  \w     94.00 136.00   1.00    5.00    --  111.00 178.00   0.00   42
 59  \w     68.00 124.00   1.00    5.00    --  111.00 178.00 150.00   56
 60  \w    -29.00  -2.00   1.00    2.00    --  -36.95 125.00  30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1206779000
_diffrn_orient_matrix_UB_12      0.0352150000
_diffrn_orient_matrix_UB_13      0.0210557000
_diffrn_orient_matrix_UB_21      0.0455878000
_diffrn_orient_matrix_UB_22      0.0370026000
_diffrn_orient_matrix_UB_23      -0.0800412000
_diffrn_orient_matrix_UB_31      -0.1098627000
_diffrn_orient_matrix_UB_32      0.1501884000
_diffrn_orient_matrix_UB_33      -0.0069849000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21826
_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         73.936
_diffrn_reflns_theta_min         4.553
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.149
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       prism
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0471P)^2^+1.2846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0834
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6775
_reflns_number_total             7474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04813d2.cif
_cod_data_source_block           kmac181(3)_scale
_cod_depositor_comments
'Adding full bibliography for 7048492--7048500.cif.'
_cod_database_code               7048494
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C36 H33 B N4 O P Ru S2 Cl3'
_reflns_odcompleteness_completeness 98.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H36,H1A,H1B} of C36
 At 1.5 times of:
  {H18A,H18B,H18C} of C18, {H14A,H14B,H14C} of C14
2.a Ternary CH refined with riding coordinates:
 C51(H51)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C16(H16),
 C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29),
  C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              78889
_ins_header
;
TITL KMAc181(3)_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.980972  11.001792  19.327890  73.7245  82.1472  65.6700
ZERR    2.00   0.000663   0.000619   0.000837   0.0044   0.0045   0.0059
LATT  1
SFAC C H B N O P S Cl Ru
UNIT 72.00 66.00 2.00 8.00 2.00 2.00 4.00 6.00 2.00
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 1.192
_oxdiff_exptl_absorpt_empirical_full_min 0.846