Furanodendralenes.
Fallon, Thomas; Willis, Anthony C; Paddon-Row, Michael N; Sherburn, Michael S; The Journal of organic chemistry 79 (2014) 3185–3193; doi:10.1021/jo500458y

data_4029220
_publ_section_title
;
 Furanodendralenes.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3185
_journal_page_last               3193
_journal_paper_doi               10.1021/jo500458y
_journal_volume                  79
_journal_year                    2014
_chemical_compound_source        local
_chemical_formula_moiety         'C38 H29 N3 O7, C3 H6 O'
_chemical_formula_sum            'C41 H35 N3 O8'
_chemical_formula_weight         697.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             13-10-15
_audit_creation_method           CRYSTALS_ver_14.40
_audit_update_record
;
2010-09    - Ian Cade collects data set cade006
2013-10-16 - Report on C41 H35 N3 O8
             by Anthony C. Willis
             for Thomas Fallon and Mick Sherburn
2013-10-16 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 109.5221(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1476(3)
_cell_length_b                   9.4116(1)
_cell_length_c                   23.5383(5)
_cell_measurement_reflns_used    30808
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     3371.58(10)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46110
_diffrn_reflns_theta_full        25.083
_diffrn_reflns_theta_max         25.083
_diffrn_reflns_theta_min         2.629
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.985
_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    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.38
_refine_ls_extinction_coef       720(60)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9617
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         5972
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.0011529
_refine_ls_shift/su_mean         0.0001380
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 2.69P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1275
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1275
_reflns_limit_h_max              18
_reflns_limit_h_min              -19
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                4708
_reflns_number_total             5972
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.24
_oxford_diffrn_Wilson_scale      8.10
_oxford_refine_ls_r_factor_ref   0.0663
_oxford_refine_ls_scale          0.3763(6)
_oxford_reflns_number_all        5972
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'she1399 At 12:45 on 15/10'
_cod_data_source_file            jo500458y_si_010.cif
_cod_data_source_block           she1399
_cod_depositor_comments
;Adding full bibliography for
 /tmp/tmp-cod-update-bibliographies-17276/cifs/4029220.cif.
;
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4029220
_iucr_refine_instruction_details_constraints
;BLOCK SCALE X'S, U'S CONT EXTPARAM RIDE C ( 2,X'S) H ( 21,X'S) RIDE C (
 3,X'S) H ( 31,X'S) RIDE C ( 7,X'S) H ( 71,X'S) RIDE C ( 8,X'S) H ( 81,X'S) H
 ( 82,X'S) RIDE C ( 9,X'S) H ( 91,X'S) RIDE C ( 10,X'S) H ( 101,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) H ( 162,X'S) RIDE C ( 17,X'S) H ( 171,X'S) RIDE C ( 21,X'S) H (
 211,X'S) RIDE C ( 22,X'S) H ( 221,X'S) RIDE C ( 27,X'S) H ( 271,X'S) RIDE C (
 28,X'S) H ( 281,X'S) RIDE C ( 29,X'S) H ( 291,X'S) RIDE C ( 30,X'S) H (
 301,X'S) RIDE C ( 31,X'S) H ( 311,X'S) RIDE C ( 35,X'S) H ( 351,X'S) RIDE C (
 36,X'S) H ( 361,X'S) RIDE C ( 37,X'S) H ( 371,X'S) RIDE C ( 38,X'S) H (
 381,X'S) RIDE C ( 39,X'S) H ( 391,X'S) RIDE C ( 43,X'S) H ( 431,X'S) RIDE C (
 44,X'S) H ( 441,X'S) RIDE C ( 45,X'S) H ( 451,X'S) RIDE C ( 46,X'S) H (
 461,X'S) RIDE C ( 47,X'S) H ( 471,X'S) RIDE C ( 51,X'S) H ( 511,X'S) H (
 512,X'S) H ( 513,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) H ( 523,X'S)
 END
;
_iucr_refine_instruction_details_restraints
;NO REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE
 THIS LINE) END
;