Computational and synthetic studies with tetravinylethylenes.
Lindeboom, Erik J.; Willis, Anthony C.; Paddon-Row, Michael N; Sherburn, Michael S.; The Journal of organic chemistry 79 (2014) 11496–11507; doi:10.1021/jo5021294

data_4030228
_publ_section_title
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 Computational and synthetic studies with tetravinylethylenes.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11496
_journal_page_last               11507
_journal_paper_doi               10.1021/jo5021294
_journal_volume                  79
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_compound_source        local
_chemical_formula_moiety         'C20 H22 N2 O4'
_chemical_formula_sum            'C20 H22 N2 O4'
_chemical_formula_weight         354.41
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-06-26
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
; 
2013-06-26 - Report on C20 H22 N2 O4 
             by Anthony C. Willis 
             for Erik J. Lindeboom and Mick Sherburn 
2013-06-26 - passes checkcif tests with minor warnings 
;
_cell_angle_alpha                90
_cell_angle_beta                 102.0128(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4676(2)
_cell_length_b                   6.9456(1)
_cell_length_c                   17.1815(4)
_cell_measurement_reflns_used    13595
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     871.64(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
; 
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20947
_diffrn_reflns_theta_full        27.466
_diffrn_reflns_theta_max         27.466
_diffrn_reflns_theta_min         2.789
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.15
_refine_ls_extinction_coef       240(30)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         2162
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.0025780
_refine_ls_shift/su_mean         0.0001867
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 0.10P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0816
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0816
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2058
_reflns_number_total             2162
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.82
_oxford_diffrn_Wilson_scale      0.42
_oxford_refine_ls_r_factor_ref   0.0324
_oxford_refine_ls_scale          1.597(12)
_oxford_reflns_number_all        2162
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'she1320 At 14:14 on 26/ 6/13'
_cod_data_source_file            jo5021294_si_005.cif
_cod_data_source_block           she1320a
_cod_depositor_comments
'Adding full bibliography for 4030223--4030230.cif.'
_cod_original_sg_symbol_Hall     'P 2yb '
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               4030228
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, C(1,U'S) UNTIL O(26) 
CONT C(6,OCC) C(106,U[ISO],OCC) 
CONT EXTPARAM 
EQUIV C(6,OCC) C(106,OCC) 
WEIGHT -1 C(106,OCC) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H(72,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) H   ( 102,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) H   ( 163,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) H   ( 243,X'S) 
RIDE C(106,X'S) H(1061,X'S) H(1062,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
DIST 1.30, .02 = C(7) TO C(106) 
ANGLE 126, 3 = C(8) TO C(7) TO C(106) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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