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_7047839
_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         'C21 H25 Cl N O5 Ru'
_chemical_formula_sum            'C21 H25 Cl N O5 Ru'
_chemical_formula_weight         507.94
_chemical_name_systematic        1b
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-12
_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                90
_cell_angle_beta                 97.680(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2589(3)
_cell_length_b                   12.7453(4)
_cell_length_c                   20.9922(5)
_cell_measurement_reflns_used    11164
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.2080
_cell_measurement_theta_min      2.5170
_cell_volume                     2189.86(12)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    8.00    --  -20.00   0.00-180.00  360
  2  \w    -51.50  14.00   0.50    8.00    --  -20.00 -72.00 108.00  131
  3  \w   -110.00  -6.50   0.50    8.00    --  -20.00   0.00 108.00  207
;
_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      0.0357971000
_diffrn_orient_matrix_UB_12      0.0042716000
_diffrn_orient_matrix_UB_13      -0.0287741000
_diffrn_orient_matrix_UB_21      0.0758030000
_diffrn_orient_matrix_UB_22      -0.0173393000
_diffrn_orient_matrix_UB_23      0.0165499000
_diffrn_orient_matrix_UB_31      -0.0219626000
_diffrn_orient_matrix_UB_32      -0.0527189000
_diffrn_orient_matrix_UB_33      -0.0077610000
_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  0.0221
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13804
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.527
_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    0.869
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79062
_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            grey
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1036
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0300P)^2^+1.2350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0627
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3451
_reflns_number_total             3804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02940g2.cif
_cod_data_source_block           1b
_cod_depositor_comments
'Adding full bibliography for 7047833--7047841.cif.'
_cod_database_code               7047839
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C23 H31 N2 O5 Ru1'
_reflns_odcompleteness_completeness 99.47
_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.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C11(H11), C14(H14), C8(H8), C19(H19), C10(H10)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              6954
_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 1.711
_oxdiff_exptl_absorpt_empirical_full_min 0.837