A novel type of organometallic 2-R-2,4-dihydro-1H-3,1-benzoxazine with R = [M(η<sup>5</sup>-C<sub>5</sub>H<sub>4</sub>)(CO)<sub>3</sub>] (M = Re or Mn) units. Experimental and computational studies of the effect of substituent R on ring-chain tautomerism.
Oyarzo, Juan; Bosque, Ramón; Toro, Patricia; Silva, Carlos P.; Arancibia, Rodrigo; Font-Bardía, Mercè; Artigas, Vania; Calvis, Carme; Messeguer, Ramon; Klahn, A. Hugo; López, Concepción; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1023–1039; doi:10.1039/c8dt03265c

data_7048357
_publ_section_title
;
 A novel type of organometallic 2-R-2,4-dihydro-1H-3,1-benzoxazine with R
 = [M(\h<sup>5</sup>-C<sub>5</sub>H<sub>4</sub>)(CO)<sub>3</sub>] (M = Re
 or Mn) units. Experimental and computational studies of the effect of
 substituent R on ring-chain tautomerism.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1023
_journal_page_last               1039
_journal_paper_doi               10.1039/c8dt03265c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C16 H12 N O4 Re'
_chemical_formula_sum            'C16 H12 N O4 Re'
_chemical_formula_weight         468.47
_chemical_melting_point          148
_chemical_name_systematic        6c
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-07-27 deposited with the CCDC.
2018-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3555(7)
_cell_length_b                   6.1536(3)
_cell_length_c                   29.7559(13)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.65
_cell_volume                     2811.7(2)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            25066
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.554
_diffrn_reflns_theta_min         2.653
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    8.661
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.5649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.213
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.031
_refine_diff_density_max         6.051
_refine_diff_density_min         -2.263
_refine_diff_density_rms         0.247
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.269(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7511
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0466P)^2^+1.0701P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.875
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.904
_reflns_number_gt                6741
_reflns_number_total             7511
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03265c2.cif
_cod_data_source_block           mo_IAGVB57_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7048356--7048358.cif.'
_cod_database_code               7048357