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_4029217
_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         'C23 H21 N3 O8, C4 H8 O2, H2 O '
_chemical_formula_sum            'C27 H31 N3 O11'
_chemical_formula_weight         573.56
_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             10-10-22
_audit_creation_method           CRYSTALS_ver_12.87
_audit_update_record
;
2010-10-22 - Report on C15 H21 N O3
             by Anthony C. Willis
             for Thomas Fallon and Mick Sherburn
2010-10-22 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90
_cell_angle_beta                 107.461(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.798(4)
_cell_length_b                   9.8024(18)
_cell_length_c                   21.099(6)
_cell_measurement_reflns_used    176337
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.6
_cell_volume                     2722.2(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 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_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  0.069
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16230
_diffrn_reflns_theta_full        25.177
_diffrn_reflns_theta_max         25.177
_diffrn_reflns_theta_min         2.591
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.78
_refine_ls_extinction_coef       220(40)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0270
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         4700
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.04
_refine_ls_shift/su_mean         0.01
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 5.18P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1971
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1971
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                2709
_reflns_number_total             4700
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.84
_oxford_diffrn_Wilson_scale      4.30
_oxford_refine_ls_r_factor_ref   0.1367
_oxford_refine_ls_scale          0.548(2)
_oxford_reflns_number_all        4700
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title '10221147 Compound X'
_cod_data_source_file            jo500458y_si_008.cif
_cod_data_source_block           she1026
_cod_depositor_comments
;The following automatic conversions were performed:

'_symmetry_cell_setting'
 value 'Monoclinic' changed to 'monoclinic'
according
 to
/usr/data/users/saulius/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 2281 2013-09-26 08:29:07Z andrius  Adding full
 bibliography for /tmp/tmp-cod-update-bibliographies-17276/cifs/4029217.cif.
;
_cod_original_cell_volume        2722.2(11)
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               4029217