A simple synthesis of [RuCl<sub>2</sub>(NHC)(p-cymene)] complexes and their use in olefin oxidation catalysis.
Ma, Xinyuan; Guillet, Sébastien G; Peng, Min; Van Hecke, Kristof; Nolan, Steven P.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 3959–3965; doi:10.1039/d1dt00030f

data_7706695
_publ_section_title
;
 A simple synthesis of [RuCl<sub>2</sub>(NHC)(p-cymene)] complexes and
 their use in olefin oxidation catalysis.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3959
_journal_page_last               3965
_journal_paper_doi               10.1039/d1dt00030f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C16 H22 N2 O3 Ru, 2(H2 O)'
_chemical_formula_sum            'C16 H26 N2 O5 Ru'
_chemical_formula_weight         427.46
_chemical_name_systematic        SN-XY-100
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-10-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-20 deposited with the CCDC.	2021-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.0610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4295(2)
_cell_length_b                   10.48900(10)
_cell_length_c                   15.6396(2)
_cell_measurement_reflns_used    8025
_cell_measurement_temperature    100.28(16)
_cell_measurement_theta_max      73.8040
_cell_measurement_theta_min      3.9690
_cell_volume                     1818.76(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.28(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.986
_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   -130.00  46.00   1.00    1.00    --  -41.68   0.00-120.00  176
  2  \w     27.00  98.00   1.00    1.00    --   41.68-125.00-180.00   71
  3  \w    -21.00  74.00   1.00    1.00    --   41.68 -77.00-150.00   95
  4  \w     33.00 132.00   1.00    1.40    --  106.01 -45.00 120.00   99
  5  \w    103.00 178.00   1.00    1.40    --  106.01  77.00-180.00   75
  6  \w     23.00 107.00   1.00    1.40    --  106.01 -94.00 120.00   84
  7  \w     33.00 112.00   1.00    1.40    --  106.01-125.00  30.00   79
  8  \w    103.00 178.00   1.00    1.40    --  106.01  77.00-150.00   75
  9  \w     33.00 112.00   1.00    1.40    --  106.01-125.00  60.00   79
 10  \w     80.00 178.00   1.00    1.40    --  106.01  45.00 -30.00   98
 11  \w   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 150.00  101
 12  \w    -33.00  66.00   1.00    1.00    --   41.68 -38.00 -60.00   99
 13  \w     14.00 115.00   1.00    1.00    --   41.68  57.00  90.00  101
 14  \w     80.00 178.00   1.00    1.40    --  106.01  45.00 150.00   98
 15  \w     77.00 178.00   1.00    1.40    --  106.01  61.00 -90.00  101
 16  \w     77.00 167.00   1.00    1.40    --  106.01  61.00  30.00   90
 17  \w     80.00 178.00   1.00    1.40    --  106.01  45.00  90.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0962237000
_diffrn_orient_matrix_UB_12      -0.0984592000
_diffrn_orient_matrix_UB_13      0.0432764000
_diffrn_orient_matrix_UB_21      0.0344472000
_diffrn_orient_matrix_UB_22      0.0834109000
_diffrn_orient_matrix_UB_23      0.0834115000
_diffrn_orient_matrix_UB_31      -0.0941015000
_diffrn_orient_matrix_UB_32      -0.0702334000
_diffrn_orient_matrix_UB_33      0.0384325000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17699
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.692
_diffrn_reflns_theta_min         3.987
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.218
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.561
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             880
_exptl_crystal_preparation       synthesis
_exptl_crystal_recrystallization_method 'hexane in cdcl3'
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         3629
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0304P)^2^+0.7171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3188
_reflns_number_total             3629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00030f2.cif
_cod_data_source_block           sn-xy-100
_cod_depositor_comments
'Adding full bibliography for 7706695--7706696.cif.'
_cod_database_code               7706695
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H26 N2 O3 RU'
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.370
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All C(H,H,H,H,H,H,H) groups
2. Restrained distances
 O5-H5A = O5-H5B
 0.84 with sigma of 0.01
 O4-H4A = O4-H4B
 0.84 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C13(H13)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C11(H11), C6(H6), C9(H9), C1(H1), C2(H2)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C3(H3A,H3B,H3C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              30002
_olex2_date_sample_data_collection 2020-10-02
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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 2.576
_oxdiff_exptl_absorpt_empirical_full_min 0.670