Structure and Reactivity of Chromium(VI) Alkylidenes.
Wu, Pengcheng; Yap, Glenn P. A.; Theopold, Klaus H.; Journal of the American Chemical Society 140 (2018) 7088–7091; doi:10.1021/jacs.8b04882

data_4132563
_publ_section_title
;
 Structure and Reactivity of Chromium(VI) Alkylidenes.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7088
_journal_page_last               7091
_journal_paper_doi               10.1021/jacs.8b04882
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C34 H52 Cr N2'
_chemical_formula_weight         540.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                72.2270(10)
_cell_angle_beta                 74.053(2)
_cell_angle_gamma                65.5810(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9722(3)
_cell_length_b                   11.1746(3)
_cell_length_c                   17.0474(4)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      74.81
_cell_measurement_theta_min      4.45
_cell_volume                     1622.84(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            41285
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.398
_diffrn_reflns_theta_min         2.763
_exptl_absorpt_coefficient_mu    3.049
_exptl_absorpt_correction_T_max  0.7539
_exptl_absorpt_correction_T_min  0.5623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX3 (Bruker, 2015)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_description       plate
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.385
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6448
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0341P)^2^+2.4789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6075
_reflns_number_total             6448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b04882_si_005.cif
_cod_data_source_block           kla0951
_cod_database_code               4132563
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.387
_shelx_estimated_absorpt_t_max   0.529
_shelx_res_checksum              68198
_shelx_hkl_checksum              33675