Hydrodeoxygenation of isocyanates: snapshots of a magnesium-mediated CO bond cleavage
Yang, Yan; Anker, Mathew D.; Fang, Jian; Mahon, Mary F.; Maron, Laurent; Weetman, Catherine; Hill, Michael S.; Chem. Sci. 8 (2017) 3529–; doi:10.1039/C7SC00117G

data_1545367
_publ_section_title
;
 Hydrodeoxygenation of isocyanates: snapshots of a magnesium-mediated
 C&#xE001;O bond cleavage
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3529
_journal_paper_doi               10.1039/C7SC00117G
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         'C35 H53 B Mg N2 O3'
_chemical_formula_sum            'C38.5 H57 B Mg N2 O3'
_chemical_formula_weight         630.98
_chemical_name_systematic
;
 ?
;
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-12 deposited with the CCDC.
2017-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1686(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   14.64625(15)
_cell_length_c                   18.8268(2)
_cell_measurement_reflns_used    8953
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      69.4100
_cell_measurement_theta_min      3.8240
_cell_volume                     3707.42(7)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22162
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
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_diffrn_reflns_theta_max         69.788
_diffrn_reflns_theta_min         3.828
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.691
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_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.235
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6916
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0632P)^2^+1.5981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5606
_reflns_number_total             6916
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc00117g2.cif
_cod_data_source_block           s16msh29_sq
_cod_depositor_comments
'Adding full bibliography for 1545365--1545370.cif.'
_cod_original_cell_volume        3707.42(8)
_cod_original_formula_sum        'C38.50 H57 B Mg N2 O3'
_cod_database_code               1545367
_shelxl_version_number           2014-3
_shelx_res_checksum              82600
_shelx_fab_checksum              73827