Highly efficient nitrogen chelated ruthenium carbene metathesis catalysts.
Duan, Yulian; Wang, Tao; Xie, Qingxiao; Yu, Xiaobo; Guo, Weijie; Wang, Jianhui; Liu, Guiyan; Dalton transactions (Cambridge, England : 2003) 45 (2016) 19441–19448; doi:10.1039/c6dt03899a

data_7041184
_publ_section_title
;
 Highly efficient nitrogen chelated ruthenium carbene metathesis
 catalysts.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19441
_journal_page_last               19448
_journal_paper_doi               10.1039/c6dt03899a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '2(C34 H38.5 Cl2 F3.5 N3 O2 Ru), 2(C H2 Cl2)'
_chemical_formula_sum            'C70 H81 Cl8 F7 N6 O4 Ru2'
_chemical_formula_weight         1689.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-09-13 deposited with the CCDC.
2016-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.710(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.0736(9)
_cell_length_b                   15.5696(6)
_cell_length_c                   16.6456(8)
_cell_measurement_reflns_used    4803
_cell_measurement_temperature    100.1(4)
_cell_measurement_theta_max      71.7370
_cell_measurement_theta_min      4.0940
_cell_volume                     3721.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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      100.1(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2740
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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      2.00  28.00   1.00   15.03    --   41.24 -99.00  90.00   26
  2  \w     26.00  97.00   1.00   15.03    --   41.24-125.00   0.00   71
  3  \w     42.00 106.00   1.00   15.03    --   41.24  38.00 -60.00   64
  4  \w     34.00  65.00   1.00   15.03    --   41.24 -99.00  90.00   31
  5  \w     26.00 103.00   1.00  102.18    --  107.08 -95.00 -60.00   77
  6  \w     88.00 177.00   1.00  102.18    --  107.08  45.00 150.00   89
  7  \w    111.00 136.00   1.00  102.18    --  107.08 -61.00   0.00   25
  8  \w    100.00 127.00   1.00  102.18    --  107.08 118.00 -18.00   27
  9  \w     36.00  62.00   1.00  102.18    --  107.08 -61.00   0.00   26
 10  \w     58.00  93.00   1.00  102.18    --  107.08-125.00-120.00   35
 11  \w   -104.00 -23.00   1.00    5.03    --  -41.49 -38.00-180.00   81
 12  \w    -37.00  -9.00   1.00    5.03    --  -41.49 125.00  30.00   28
 13  \w     71.00 100.00   1.00   52.18    --  107.08 -95.00-120.00   29
 14  \w     28.00  55.00   1.00   52.18    --  107.08 -95.00-120.00   27
 15  \w    152.00 177.00   1.00   52.18    --  107.08 125.00 150.00   25
 16  \w     95.00 131.00   1.00   52.18    --  107.08 125.00 150.00   36
 17  \w     42.00  92.00   1.00   52.18    --  107.08 -61.00  30.00   50
 18  \w     99.00 144.00   1.00   52.18    --  107.08 125.00 -90.00   45
 19  \w    137.00 170.00   1.00   52.18    --  107.08  61.00 -30.00   33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0944282000
_diffrn_orient_matrix_UB_12      0.0464550000
_diffrn_orient_matrix_UB_13      0.0362173000
_diffrn_orient_matrix_UB_21      0.0509588000
_diffrn_orient_matrix_UB_22      -0.0863022000
_diffrn_orient_matrix_UB_23      0.0339750000
_diffrn_orient_matrix_UB_31      0.0016092000
_diffrn_orient_matrix_UB_32      -0.0136072000
_diffrn_orient_matrix_UB_33      -0.0909449000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0952
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16049
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         4.111
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.504
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.961
_refine_diff_density_min         -1.029
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0564P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1276
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5117
_reflns_number_total             6616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03899a2.cif
_cod_data_source_block           a160311c
_cod_depositor_comments          'Adding full bibliography for 7041184.cif.'
_cod_database_code               7041184
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H28(0.5) F3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C22(H22A,H22B), C23(H23A,H23B), C33(H33A,
 H33B), C35(H35A,H35B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C17(H17), C26(H26), C27(H27), C28(H28), C29(H29)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C34(H34A,H34B,H34C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-03-14
_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 2.372
_oxdiff_exptl_absorpt_empirical_full_min 0.599