Diverse modes of functionalisation of ruthenium coordinated β-ketoiminate analogues.
Bera, Sudip Kumar; Panda, Sanjib; Dey Baksi, Sourajit; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15897–15906; doi:10.1039/c8dt02940g

data_7047835
_publ_section_title
;
 Diverse modes of functionalisation of ruthenium coordinated
 \b-ketoiminate analogues.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15897
_journal_page_last               15906
_journal_paper_doi               10.1039/c8dt02940g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '2(C22 H28 N O6 Ru)'
_chemical_formula_sum            'C44 H56 N2 O12 Ru2'
_chemical_formula_weight         1007.04
_chemical_name_systematic        1c
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-04 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                107.603(10)
_cell_angle_beta                 97.419(9)
_cell_angle_gamma                90.534(8)
_cell_formula_units_Z            2
_cell_length_a                   11.3588(12)
_cell_length_b                   12.8458(13)
_cell_length_c                   15.7582(18)
_cell_measurement_reflns_used    3257
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.3520
_cell_measurement_theta_min      1.8000
_cell_volume                     2170.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -110.00  70.00   0.50   16.00    --  -20.00   0.00-180.00  360
  2  \w    -71.00   8.00   0.50   16.00    --  -20.00 -72.00 -36.00  158
  3  \w    -78.00   5.00   0.50   16.00    --  -20.00 -72.00-180.00  166
  4  \w    -53.00   1.00   0.50   16.00    --  -20.00  72.00 108.00  108
  5  \w    -59.00 -35.00   0.50   16.00    --  -20.00  72.00 -36.00   48
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0171329000
_diffrn_orient_matrix_UB_12      0.0549003000
_diffrn_orient_matrix_UB_13      0.0102427000
_diffrn_orient_matrix_UB_21      -0.0085469000
_diffrn_orient_matrix_UB_22      -0.0048643000
_diffrn_orient_matrix_UB_23      -0.0464559000
_diffrn_orient_matrix_UB_31      -0.0600773000
_diffrn_orient_matrix_UB_32      -0.0180801000
_diffrn_orient_matrix_UB_33      -0.0032395000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1443
_diffrn_reflns_av_unetI/netI     0.2052
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16870
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.810
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41439
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1036
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.838
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1611
_refine_ls_R_factor_gt           0.0946
_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^)+(0.0642P)^2^+2.5460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4503
_reflns_number_total             7658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02940g2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 7047833--7047841.cif.'
_cod_database_code               7047835
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C41 H55 N5 O12 Ru2'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(C13) = Uanis(C14)
Uanis(C3) = Uanis(C2)
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C33(H33), C29(H29), C32(H32), C7(H7), C36(H36), C25(H25), C10(H10),
 C3(H3), C30(H30), C19(H19), C41(H41), C8(H8), C11(H11)
3.b Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C16(H16A,H16B,H16C), C5(H5A,H5B,H5C), C38(H38A,H38B,
 H38C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C27(H27A,
 H27B,H27C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C1(H1A,H1B,H1C),
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              84023
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.358
_oxdiff_exptl_absorpt_empirical_full_min 0.464