#------------------------------------------------------------------------------
#$Date: 2020-09-06 10:39:25 +0200 (dom 06 de sep de 2020) $
#$Revision: 256033 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/68/7126839.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7126839
loop_
_publ_author_name
'Yakiyama, Yumi'
'Fujinaka, Takahisa'
'Nishimura, Mio'
'Seki, Ryotaro'
'Sakurai, Hidehiro'
_publ_section_title
;
 Control by one drop of solvent: selective preparation of guest
 release/trap-triggered interconvertible molecular crystals.
;
_journal_issue                   67
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9687
_journal_page_last               9690
_journal_paper_doi               10.1039/d0cc03408h
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C28 H16 N2 O4'
_chemical_formula_sum            'C28 H16 N2 O4'
_chemical_formula_weight         444.43
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-16 deposited with the CCDC.	2020-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.9380(8)
_cell_length_b                   15.9380(8)
_cell_length_c                   15.9529(7)
_cell_measurement_reflns_used    6966
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.6140
_cell_measurement_theta_min      2.5520
_cell_volume                     4052.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.817
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     17.00  42.00   0.50   36.06    --    5.18  88.00  16.00   50
  2  ω    -23.00  14.00   0.50   36.06    --   -5.26 -88.00 -99.00   74
  3  ω    -23.00  39.00   0.50   36.06    --    5.18 -99.00  60.00  124
  4  ω     -9.00  28.00   0.50   36.06    --   -5.26 -99.00 120.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0022787000
_diffrn_orient_matrix_UB_12      0.0277359000
_diffrn_orient_matrix_UB_13      -0.0347760000
_diffrn_orient_matrix_UB_21      0.0545718000
_diffrn_orient_matrix_UB_22      0.0500670000
_diffrn_orient_matrix_UB_23      0.0486726000
_diffrn_orient_matrix_UB_31      0.0312511000
_diffrn_orient_matrix_UB_32      -0.0261439000
_diffrn_orient_matrix_UB_33      -0.0192962000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.817
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11489
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.735
_diffrn_reflns_theta_min         2.556
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0492P)²+2.5550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2249
_reflns_number_total             2574
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc03408h2.cif
_cod_data_source_block           1a-EtOAc
_cod_depositor_comments
'Adding full bibliography for 7126838--7126851.cif.'
_cod_original_cell_volume        4052.4(4)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7126839
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.973
_reflns_odcompleteness_completeness 80.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14)
;
_olex2_exptl_crystal_mounting_method Litholoop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.163
_oxdiff_exptl_absorpt_empirical_full_min 0.857
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.39214(5) 0.69383(5) 0.47691(5) 0.02284(19) Uani 1 1 d . . . . .
O2 O 0.64486(5) 0.67211(5) 0.32191(5) 0.02268(19) Uani 1 1 d . . . . .
N1 N 0.36597(6) 0.57736(6) 0.16288(6) 0.0243(2) Uani 1 1 d . . . . .
C1 C 0.49975(6) 0.70033(6) 0.36727(6) 0.0157(2) Uani 1 1 d . . . . .
C2 C 0.46062(6) 0.67229(7) 0.45204(6) 0.0171(2) Uani 1 1 d . . . . .
C3 C 0.52216(7) 0.62059(6) 0.49799(7) 0.0180(2) Uani 1 1 d . . . . .
C4 C 0.51414(7) 0.58442(7) 0.57684(7) 0.0211(2) Uani 1 1 d . . . . .
H4 H 0.463742 0.589342 0.608254 0.025 Uiso 1 1 calc R . . . .
C5 C 0.58299(8) 0.54070(7) 0.60785(7) 0.0236(2) Uani 1 1 d . . . . .
H5 H 0.579760 0.515467 0.661697 0.028 Uiso 1 1 calc R . . . .
C6 C 0.65686(8) 0.53323(7) 0.56121(8) 0.0249(3) Uani 1 1 d . . . . .
H6 H 0.702216 0.501447 0.583234 0.030 Uiso 1 1 calc R . . . .
C7 C 0.66536(7) 0.57129(7) 0.48333(7) 0.0224(2) Uani 1 1 d . . . . .
H7 H 0.716117 0.567387 0.452345 0.027 Uiso 1 1 calc R . . . .
C8 C 0.59654(7) 0.61539(6) 0.45247(7) 0.0186(2) Uani 1 1 d . . . . .
C9 C 0.59004(6) 0.66393(6) 0.37363(6) 0.0173(2) Uani 1 1 d . . . . .
C10 C 0.32659(7) 0.60598(7) 0.23132(7) 0.0215(2) Uani 1 1 d . . . . .
H10 H 0.267663 0.597776 0.234974 0.026 Uiso 1 1 calc R . . . .
C11 C 0.36608(7) 0.64681(7) 0.29726(7) 0.0194(2) Uani 1 1 d . . . . .
H11 H 0.334658 0.665290 0.344379 0.023 Uiso 1 1 calc R . . . .
C12 C 0.45250(6) 0.66041(6) 0.29353(6) 0.0165(2) Uani 1 1 d . . . . .
C13 C 0.49404(7) 0.63201(7) 0.22214(7) 0.0216(2) Uani 1 1 d . . . . .
H13 H 0.552727 0.640481 0.216058 0.026 Uiso 1 1 calc R . . . .
C14 C 0.44863(8) 0.59107(7) 0.15979(8) 0.0253(2) Uani 1 1 d . . . . .
H14 H 0.478331 0.571637 0.111947 0.030 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 N1 C10 115.87(10) . . ?
C2 C1 C1 106.82(6) . 6_564 ?
C2 C1 C9 101.96(8) . . ?
C9 C1 C1 111.62(10) . 6_564 ?
C12 C1 C1 114.64(7) . 6_564 ?
C12 C1 C2 110.52(8) . . ?
C12 C1 C9 110.46(8) . . ?
O1 C2 C1 124.41(9) . . ?
O1 C2 C3 126.47(10) . . ?
C3 C2 C1 109.02(8) . . ?
C4 C3 C2 128.32(10) . . ?
C4 C3 C8 121.71(10) . . ?
C8 C3 C2 109.87(9) . . ?
C3 C4 C5 117.20(10) . . ?
C4 C5 C6 121.20(10) . . ?
C7 C6 C5 121.39(10) . . ?
C6 C7 C8 117.37(11) . . ?
C3 C8 C9 110.63(9) . . ?
C7 C8 C3 121.07(10) . . ?
C7 C8 C9 128.26(10) . . ?
O2 C9 C1 125.74(9) . . ?
O2 C9 C8 125.86(9) . . ?
C8 C9 C1 108.37(8) . . ?
N1 C10 C11 124.40(10) . . ?
C10 C11 C12 119.22(10) . . ?
C11 C12 C1 121.06(9) . . ?
C13 C12 C1 121.88(9) . . ?
C13 C12 C11 116.97(10) . . ?
C14 C13 C12 119.30(10) . . ?
N1 C14 C13 124.24(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C2 1.2110(12) . ?
O2 C9 1.2087(13) . ?
N1 C10 1.3394(15) . ?
N1 C14 1.3364(16) . ?
C1 C1 1.583(2) 6_564 ?
C1 C2 1.5549(14) . ?
C1 C9 1.5549(14) . ?
C1 C12 1.5347(14) . ?
C2 C3 1.4759(14) . ?
C3 C4 1.3897(15) . ?
C3 C8 1.3926(15) . ?
C4 C5 1.3907(15) . ?
C5 C6 1.3978(17) . ?
C6 C7 1.3892(17) . ?
C7 C8 1.3927(14) . ?
C8 C9 1.4802(14) . ?
C10 C11 1.3880(15) . ?
C11 C12 1.3956(14) . ?
C12 C13 1.3929(15) . ?
C13 C14 1.3925(16) . ?
