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_4030229
_publ_section_title
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 Computational and synthetic studies with tetravinylethylenes.
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_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         'C28 H30 O12'
_chemical_formula_sum            'C28 H30 O12'
_chemical_formula_weight         558.54
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             12-11-06
_audit_creation_method           CRYSTALS_ver_14.11
_audit_update_record
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2012-11-06 - Report on C28 H30 O12 
             by Anthony C. Willis 
             for Erik J. Lindeboom and Mick Sherburn 
2012-11-07 - passes checkcif tests with minor warnings 
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4837(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3961(2)
_cell_length_b                   15.5192(5)
_cell_length_c                   16.7740(4)
_cell_measurement_reflns_used    100454
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2705.40(12)
_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 & \w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50270
_diffrn_reflns_theta_full        27.499
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.625
_diffrn_standards_number         0
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_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1176.000
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         6210
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_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.0097737
_refine_ls_shift/su_mean         0.0003331
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 1.14P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1324
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1324
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4282
_reflns_number_total             6211
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.83
_oxford_diffrn_Wilson_scale      6.88
_oxford_refine_ls_r_factor_ref   0.0839
_oxford_refine_ls_scale          0.4343(7)
_oxford_reflns_number_all        6210
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '11061242 she1237'
_cod_data_source_file            jo5021294_si_009.cif
_cod_data_source_block           she1237
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4030223--4030230.cif.
;
_cod_original_sg_symbol_H-M      'P 1 21/a 1 '
_cod_database_code               4030229
_iucr_refine_instruction_details_constraints
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BLOCK SCALE C(1,X'S, U'S) UNTIL C(40) 
CONT C(101,X'S,U[ISO],OCC) UNTIL C(102) C(1,OCC) C(2,OCC) 
EQUIV C(1,OCC) C(2,OCC) C(101,OCC) C(102,OCC) 
WEIGHT -1 C(101,OCC) C(102,OCC) 
FIX C(101,U[ISO]) UNTIL C(102) 
RIDE C   (   1,X'S) H   (  11,X'S) H   (  12,X'S) 
RIDE C   (   2,X'S) H   (  22,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) H(32,X'S) 
RIDE C   (   6,X'S) H   (  62,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 112,X'S) H   ( 111,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H(142,X'S) 
RIDE C   (  20,X'S) H   ( 202,X'S) H   ( 201,X'S) H   ( 203,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 243,X'S) H   ( 242,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) H   ( 283,X'S) H   ( 282,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) H   ( 322,X'S) H   ( 323,X'S) 
RIDE C   (  36,X'S) H   ( 362,X'S) H   ( 361,X'S) H   ( 363,X'S) 
RIDE C   (  40,X'S) H   ( 402,X'S) H   ( 401,X'S) H   ( 403,X'S) 
RIDE C(101,X'S) H(1011,X'S) H(1012,X'S) 
RIDE C(102,X'S) H(1021,X'S) H(1022,X'S) 
END                                                                             
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_iucr_refine_instruction_details_restraints
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DIST 1.54, .02 = C(14) TO C(101) 
DIST 1.51, .02 = C(101) TO C(102) 
DIST 1.53, .02 = C(102) TO C(3) 
ANGLE 110, 2 = C(14) TO C(101) TO C(102) 
ANGLE 112, 2 = C(101) TO C(102) TO C(3) 
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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