Selective Deoxygenation of Nitrate to Nitrosyl using Trivalent Chromium and the Mashima Reagent: Reductive Silylation
Seo, Junghee; Cabelof, Alyssa; Chen, Chun-Hsing; Caulton, Kenneth G.; Chemical Science  (2019) –; doi:10.1039/C8SC02979B

data_1550039
_publ_section_title
;
 Selective Deoxygenation of Nitrate to Nitrosyl using Trivalent Chromium
 and the Mashima Reagent: Reductive Silylation
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC02979B
_journal_year                    2019
_chemical_formula_moiety         'C27 H41 Cr1 N8 O9'
_chemical_formula_sum            'C27 H41 Cr N8 O9'
_chemical_formula_weight         673.67
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-27
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_audit_update_record
;
2018-06-11 deposited with the CCDC.
2018-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.791(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.214(13)
_cell_length_b                   10.381(4)
_cell_length_c                   23.797(10)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    100
_cell_measurement_theta_max      14
_cell_measurement_theta_min      2
_cell_volume                     6830(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_type            'CMOS pixel array detector'
_diffrn_measured_fraction_theta_full 0.519
_diffrn_measured_fraction_theta_max 0.515
_diffrn_measurement_device       'huber three-circle diffractometer'
_diffrn_measurement_device_type  'Pilatus1M(CdTe) pixel array detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'silicon  1 1 1 and 3 1 1'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26934
_diffrn_reflns_theta_full        11.977
_diffrn_reflns_theta_max         15.554
_diffrn_reflns_theta_min         1.079
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.33
_refine_diff_density_min         -1.15
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         5908
_refine_ls_number_restraints     90
_refine_ls_R_factor_all          0.1539
_refine_ls_R_factor_gt           0.1283
_refine_ls_shift/su_max          0.0174473
_refine_ls_shift/su_mean         0.0010238
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 17.7 26.8 12.0 2.72 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3578
_refine_ls_wR_factor_gt          0.3321
_refine_ls_wR_factor_ref         0.3578
_reflns_limit_h_max              35
_reflns_limit_h_min              -39
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              0
_reflns_number_gt                4254
_reflns_number_total             5931
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.82
_oxford_diffrn_Wilson_scale      649.66
_oxford_refine_ls_r_factor_ref   0.1538
_oxford_refine_ls_scale          0.04389(2)
_oxford_reflns_number_all        5909
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 's18001 in C2/c'
_cod_data_source_file            c8sc02979b2.cif
_cod_data_source_block           S18001
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C27 H41 Cr1 N8 O9'
_cod_database_code               1550039