Electrochemically Mediated Oxidative Transformations of Substituted 4-Methoxystilbenes: Effect of Ortho-Substituted Nucleophilic Groups.
Chong, Kam-Weng; Hong, Fong-Jiao; Thomas, Noel F.; Low, Yun-Yee; Kam, Toh-Seok; The Journal of organic chemistry 82 (2017) 6172–6191; doi:10.1021/acs.joc.7b00753

data_4032568
_publ_section_title
;
 Electrochemically Mediated Oxidative Transformations of Substituted
 4-Methoxystilbenes: Effect of Ortho-Substituted Nucleophilic Groups.
;
_journal_issue                   12
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6172
_journal_page_last               6191
_journal_paper_doi               10.1021/acs.joc.7b00753
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C46 H44 N2 O8 S2, C H4 O'
_chemical_formula_sum            'C47 H48 N2 O9 S2'
_chemical_formula_weight         848.99
_chemical_melting_point          189.0(10)
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 107.310(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9497(3)
_cell_length_b                   42.7991(18)
_cell_length_c                   11.4651(4)
_cell_measurement_reflns_used    7271
_cell_measurement_temperature    147(1)
_cell_measurement_theta_max      72.7430
_cell_measurement_theta_min      4.1080
_cell_volume                     4192.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material
'enCIFer (Allen, et. al., J. Applied Cryst., 37, 335-338, 2004)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(1)
_diffrn_detector_area_resol_mean 5.2020
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.015
_diffrn_reflns_theta_min         4.132
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.648
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     1097
_refine_ls_number_reflns         12298
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+9.8429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1810
_refine_ls_wR_factor_ref         0.1840
_reflns_Friedel_coverage         0.973
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                11476
_reflns_number_total             12298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b00753_si_015.cif
_cod_data_source_block           exp_6125
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '188-190' was changed to '189.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 4032566--4032573.cif.

2020-08-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     'C94 H96 N4 O18 S4'
_cod_original_formula_sum        'C94 H96 N4 O18 S4'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1697.98
_cod_database_code               4032568
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              69794
_shelx_hkl_checksum              16132