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_4030227
_publ_section_title
;
 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_compound_source        local
_chemical_formula_moiety         'C34 H28'
_chemical_formula_sum            'C34 H28'
_chemical_formula_weight         436.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             13-07-04
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
; 
2013-07-08 - Report on C34 H28 
             by Anthony C. Willis 
             for Erik J. Lindeboom and Mick Sherburn 
2013-07-09 - passes checkcif tests with minor warnings 
;
_cell_angle_alpha                90
_cell_angle_beta                 93.1287(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4959(2)
_cell_length_b                   7.4350(1)
_cell_length_c                   24.6097(3)
_cell_measurement_reflns_used    51930
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2465.71(6)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.051
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            46744
_diffrn_reflns_theta_full        27.484
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.862
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             928.000
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9678
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         5641
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0583
_refine_ls_shift/su_max          0.0106050
_refine_ls_shift/su_mean         0.0010028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 1.07P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1532
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1532
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                4098
_reflns_number_total             5641
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.89
_oxford_diffrn_Wilson_scale      1.71
_oxford_refine_ls_r_factor_ref   0.0810
_oxford_refine_ls_scale          0.866(3)
_oxford_reflns_number_all        5641
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'she1311a At 12:15 on 22/ 5'
_cod_data_source_file            jo5021294_si_002.cif
_cod_data_source_block           she1311a
_cod_depositor_comments
'Adding full bibliography for 4030223--4030230.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4030227
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S 
CONT C(1,U'S) UNTIL C(5), C(6,U'S,OCC) UNTIL C(10) 
CONT C(11,U'S) UNTIL C(22) 
CONT  C(23,U'S,OCC)   UNTIL C(34) 
CONT  C(106,U[ISO],OCC) UNTIL C(134) 
EQUIV C(6,OCC)  UNTIL C(10) 
CONT  C(23,OCC)  UNTIL C(34) 
CONT C(106,OCC) UNTIL C(134) 
WEIGHT -1 C(106,OCC) UNTIL C(134) 
EQUIV  C(123,U[ISO]) UNTIL C(128) 
EQUIV  C(129,U[ISO]) UNTIL C(134) 
RIDE C ( 1,X'S) H( 11,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) 
RIDE C(6,X'S) H(61,X'S) 
RIDE C(7,X'S) H(71,X'S) 
RIDE C(9,X'S) H(91,X'S) 
RIDE C(10,X'S) H(101,X'S) 
RIDE C ( 12,X'S) H( 121,X'S) 
RIDE C ( 13,X'S) H( 131,X'S) 
RIDE C ( 14,X'S) H( 141,X'S) 
RIDE C ( 15,X'S) H( 151,X'S) 
RIDE C ( 16,X'S) H( 161,X'S) 
RIDE C ( 18,X'S) H( 181,X'S) 
RIDE C ( 19,X'S) H( 191,X'S) 
RIDE C ( 20,X'S) H( 201,X'S) 
RIDE C ( 21,X'S) H( 211,X'S) 
RIDE C ( 22,X'S) H( 221,X'S) 
RIDE C ( 24,X'S) H( 241,X'S) 
RIDE C ( 25,X'S) H( 251,X'S) 
RIDE C ( 26,X'S) H( 261,X'S) 
RIDE C ( 27,X'S) H( 271,X'S) 
RIDE C ( 28,X'S) H( 281,X'S) 
RIDE C ( 30,X'S) H( 301,X'S) 
RIDE C ( 31,X'S) H( 311,X'S) 
RIDE C ( 32,X'S) H( 321,X'S) 
RIDE C ( 33,X'S) H( 331,X'S) 
RIDE C ( 34,X'S) H( 341,X'S) 
RIDE C(106,X'S) H(1061,X'S) 
RIDE C(107,X'S) H(1071,X'S) 
RIDE C(109,X'S) H(1091,X'S) 
RIDE C(110,X'S) H(1101,X'S) 
RIDE C ( 124,X'S) H( 1241,X'S) 
RIDE C ( 125,X'S) H( 1251,X'S) 
RIDE C ( 126,X'S) H( 1261,X'S) 
RIDE C ( 127,X'S) H( 1271,X'S) 
RIDE C ( 128,X'S) H( 1281,X'S) 
RIDE C ( 130,X'S) H( 1301,X'S) 
RIDE C ( 131,X'S) H( 1311,X'S) 
RIDE C ( 132,X'S) H( 1321,X'S) 
RIDE C ( 133,X'S) H( 1331,X'S) 
RIDE C ( 134,X'S) H( 1341,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
DIST 1.37, .02 = C(3) TO C(108) 
DIST 1.48, .02 = C(108) TO C(107), C(108) TO C(109) 
DIST 1.35, .02 = C(106) TO C(107), C(109) TO C(110) 
DIST 1.48, .02 = C(106) TO C(123), C(110) TO C(129) 
DIST 1.42, .02 = C(123) TO C(124), C(123) TO C(128), C(124) TO C(125) 
CONT             C(125) TO C(126), C(126) TO C(127), C(127) TO C(128) 
DIST 1.42, .02 = C(129) TO C(130), C(129) TO C(134), C(130) TO C(131) 
CONT             C(131) TO C(132), C(132) TO C(133), C(133) TO C(134) 
PLANAR C(123) UNTIL C(128) 
PLANAR C(129) UNTIL C(134) 
ANGLE 122, 2 = C(107) TO C(108) TO C(109) 
ANGLE 125, 2 = C(106) TO C(107) TO C(108), C(108) TO C(109) TO C(110) 
ANGLE 124, 2 = C(107) TO C(106) TO C(123), C(109) TO C(110) TO C(129) 
REM 
ANGLE 120 3 = C(106) TO C(123) TO C(124), C(106) TO C(123) TO C(128) 
ANGLE 120 3 = C(128) TO C(123) TO C(124), C(123) TO C(124) TO C(125) 
CONT C(124) TO C(125) TO C(125), C(125) TO C(126) TO C(127) 
CONT C(126) TO C(127) TO C(128), C(127) TO C(128) TO C(123) 
REM 
ANGLE 120 3 = C(110) TO C(129) TO C(130), C(110) TO C(129) TO C(130) 
ANGLE 120 3 =  C(134) TO C(129) TO C(130), C(129) TO C(130) TO C(131) 
CONT C(130) TO C(131) TO C(132), C(131) TO C(132) TO C(133) 
CONT C(132) TO C(133) TO C(134), C(133) TO C(134) TO C(129) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;