Environment-Sensitive Azepane-Substituted β-Diketones and Difluoroboron Complexes with Restricted C–C Bond Rotation
Wang, Fang; DeRosa, Christopher A.; Song, Daniel; Dickie, Diane A.; Fraser, Cassandra L.; The Journal of Physical Chemistry C 123 (2019) 23124–; doi:10.1021/acs.jpcc.9b06304

data_1554146
_publ_section_title
;
 Environment-Sensitive Azepane-Substituted \b-Diketones and Difluoroboron
 Complexes with Restricted C--C Bond Rotation
;
_journal_issue                   37
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              23124
_journal_paper_doi               10.1021/acs.jpcc.9b06304
_journal_volume                  123
_journal_year                    2019
_chemical_formula_sum            'C22 H23 N O2'
_chemical_formula_weight         333.41
_chemical_name_common            L-Strap
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 104.310(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.715(7)
_cell_length_b                   13.139(6)
_cell_length_c                   17.882(12)
_cell_measurement_reflns_used    1860
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      24.4316
_cell_measurement_theta_min      2.3509
_cell_volume                     3350(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker Instrument Service v2017.5.0.0'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII Duo'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1708
_diffrn_reflns_av_unetI/netI     0.1355
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25106
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.95
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.780
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1565
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0794P)^2^+0.5736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1673
_refine_ls_wR_factor_ref         0.2163
_reflns_number_gt                1565
_reflns_number_total             3181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp9b06304_si_002.cif
_cod_data_source_block           Fraser_FW_LStrap1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3350.(3)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               1554146
_shelx_res_checksum              16852
_shelx_hkl_checksum              72218