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_7048493
_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         'C27 H27 Cl2 N4 O P Ru S2'
_chemical_formula_sum            'C27 H27 Cl2 N4 O P Ru S2'
_chemical_formula_weight         690.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-03
_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                90
_cell_angle_beta                 94.733(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2352(4)
_cell_length_b                   16.5996(6)
_cell_length_c                   18.7713(7)
_cell_measurement_reflns_used    5801
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.7830
_cell_measurement_theta_min      4.0820
_cell_volume                     2867.84(19)
_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 0.997
_diffrn_measured_fraction_theta_max 0.871
_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    -11.00  83.00   1.00   60.04    --   15.42  77.00 -90.00   94
  2  \w      4.00  54.00   1.00   60.04    --   15.42 -99.00  60.00   50
  3  \w    -50.00  42.00   1.00   60.04    --   15.42 -77.00 150.00   92
  4  \w    -40.00  38.00   1.00   60.04    --   15.42 -19.00 -30.00   78
;
_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      -0.0420954000
_diffrn_orient_matrix_UB_12      -0.0322096000
_diffrn_orient_matrix_UB_13      0.0120231000
_diffrn_orient_matrix_UB_21      0.0585691000
_diffrn_orient_matrix_UB_22      -0.0269029000
_diffrn_orient_matrix_UB_23      -0.0038748000
_diffrn_orient_matrix_UB_31      0.0273802000
_diffrn_orient_matrix_UB_32      0.0079905000
_diffrn_orient_matrix_UB_33      0.0357193000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            9934
_diffrn_reflns_point_group_measured_fraction_full 0.832
_diffrn_reflns_point_group_measured_fraction_max 0.693
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.326
_diffrn_reflns_theta_min         3.456
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67806
_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    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 1843 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.017(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5442
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.1202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.589
_reflns_Friedel_fraction_full    0.667
_reflns_Friedel_fraction_max     0.515
_reflns_number_gt                5212
_reflns_number_total             5442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04813d2.cif
_cod_data_source_block           kmac185(1)
_cod_depositor_comments
'Adding full bibliography for 7048492--7048500.cif.'
_cod_database_code               7048493
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C27H27RuN4S2BOPCl
_reflns_odcompleteness_completeness 99.54
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), 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.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              78436
_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 1.383
_oxdiff_exptl_absorpt_empirical_full_min 0.732