Reactivity and Selectivity in Catalytic Reactions of Enoldiazoacetamides. Assessment of Metal Carbenes as Intermediates
Deng, Yongming; Jing, Changcheng; Arman, Hadi; Doyle, Michael P.; Organometallics 35 (2016) 3413–; doi:10.1021/acs.organomet.6b00648

data_4089026
_publ_section_title
;
 Reactivity and Selectivity in Catalytic Reactions of Enoldiazoacetamides.
 Assessment of Metal Carbenes as Intermediates
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              3413
_journal_paper_doi               10.1021/acs.organomet.6b00648
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C33 H42 Cl2 O3 Ru Si'
_chemical_formula_sum            'C33 H42 Cl2 O3 Ru Si'
_chemical_formula_weight         686.72
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.288(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1410(15)
_cell_length_b                   15.406(2)
_cell_length_c                   21.056(3)
_cell_measurement_reflns_used    12507
_cell_measurement_temperature    298
_cell_measurement_theta_max      40.2
_cell_measurement_theta_min      2.4
_cell_volume                     3275.6(8)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
	Number of images: 246
	           Slice: -68.0000 - 55.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 70.0000
	             Phi: 180.0000
	             XTD: 34.9548
	          2theta: -34.9827
scan:
	Number of images: 202
	           Slice: -67.0000 - 34.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 70.0000
	             Phi: 0.0000
	             XTD: 34.9548
	          2theta: -34.9827
scan:
	Number of images: 140
	           Slice: -90.0000 - -20.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 180.0000
	             XTD: 34.9548
	          2theta: -34.9827
scan:
	Number of images: 60
	           Slice: -115.0000 - -85.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 270.0000
	             XTD: 34.9548
	          2theta: -34.9827
scan:
	Number of images: 54
	           Slice: -61.0000 - -34.0000
	     Image width: 0.5000
	        Exp time: 45.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 70.0000
	             Phi: 270.0000
	             XTD: 34.9548
	          2theta: -34.9827
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn724 (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.009700
_diffrn_orient_matrix_UB_12      0.065290
_diffrn_orient_matrix_UB_13      0.073826
_diffrn_orient_matrix_UB_21      0.064595
_diffrn_orient_matrix_UB_22      0.003713
_diffrn_orient_matrix_UB_23      0.005204
_diffrn_orient_matrix_UB_31      0.000054
_diffrn_orient_matrix_UB_32      0.038503
_diffrn_orient_matrix_UB_33      -0.028148
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21737
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.498
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.318
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Higashi, 1995)'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.902
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0510P)^2^+1.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5512
_reflns_number_total             6095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00648_si_002.cif
_cod_data_source_block           cd1332a
_cod_database_code               4089026
_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.a Ternary CH refined with riding coordinates:
 C11(H11), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.c Aromatic/amide H refined with riding coordinates:
 C29(H29), C30(H30), C13(H13), C2(H2), C26(H26), C17(H17), C27(H27), C16(H16),
 C6(H6), C14(H14), C15(H15), C4(H4), C3(H3), C5(H5)
2.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C19(H19A,H19B,H19C), C33(H33A,H33B,
 H33C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C21(H21A,
 H21B,H21C)
;
_shelx_res_checksum              5474
_shelx_hkl_checksum              60700
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'