#------------------------------------------------------------------------------
#$Date: 2021-10-06 18:33:10 +0300 (Wed, 06 Oct 2021) $
#$Revision: 269708 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708115.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_7708115
loop_
_publ_author_name
'Matos, Catiúcia R M O'
'Sanii, Rana'
'Wang, Shi-Qiang'
'Ronconi, Célia M'
'Zaworotko, Michael J.'
_publ_section_title
;
 Reversible single-crystal to single-crystal phase transformation between
 a new Werner clathrate and its apohost.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12923
_journal_page_last               12930
_journal_paper_doi               10.1039/d1dt01839f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C17 H10 N2 O2'
_chemical_formula_sum            'C17 H10 N2 O2'
_chemical_formula_weight         274.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-07 deposited with the CCDC.	2021-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   3.8466(2)
_cell_length_b                   15.6309(6)
_cell_length_c                   20.3882(8)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      33.14
_cell_measurement_theta_min      2.61
_cell_volume                     1225.86(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      105.82
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29701
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.488
_diffrn_reflns_theta_min         2.791
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0563 before and 0.0525 after correction. The Ratio of minimum to maximum transmission is 0.9573. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 944 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0295
_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)+(0.0415P)²+0.3430P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.651
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2448
_reflns_number_total             2533
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01839f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7708105--7708117.cif.'
_cod_database_code               7708115
_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
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H),
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
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
O001 O 0.9303(3) 0.64234(8) 0.47468(6) 0.0177(3) Uani 1 1 d . . . . .
O002 O 0.3640(4) 0.49826(8) 0.31208(6) 0.0218(3) Uani 1 1 d . . . . .
N003 N 0.6570(4) 0.56848(9) 0.39305(7) 0.0147(3) Uani 1 1 d . . . . .
N004 N 0.7511(4) 0.34457(10) 0.44840(8) 0.0207(3) Uani 1 1 d . . . . .
C005 C 0.7464(5) 0.71005(11) 0.30826(8) 0.0141(3) Uani 1 1 d . . . . .
C006 C 0.8596(5) 0.71562(11) 0.37395(8) 0.0146(4) Uani 1 1 d . . . . .
C007 C 0.5233(5) 0.56160(11) 0.32882(8) 0.0148(4) Uani 1 1 d . . . . .
C008 C 0.8236(5) 0.64185(11) 0.41868(8) 0.0139(3) Uani 1 1 d . . . . .
C009 C 0.5849(5) 0.63513(11) 0.28453(8) 0.0150(4) Uani 1 1 d . . . . .
C00A C 0.7932(5) 0.78109(11) 0.26564(9) 0.0166(4) Uani 1 1 d . . . . .
C00B C 0.6324(5) 0.49418(11) 0.43516(8) 0.0149(4) Uani 1 1 d . . . . .
C00C C 0.9533(5) 0.85611(12) 0.29083(9) 0.0192(4) Uani 1 1 d . . . . .
H00C H 0.986605 0.904155 0.262997 0.023 Uiso 1 1 calc R . . . .
C00D C 0.5238(5) 0.70014(12) 0.17775(9) 0.0198(4) Uani 1 1 d . . . . .
H00D H 0.449192 0.696345 0.133424 0.024 Uiso 1 1 calc R . . . .
C00E C 1.0601(5) 0.85986(11) 0.35484(9) 0.0201(4) Uani 1 1 d . . . . .
H00E H 1.165463 0.910633 0.370981 0.024 Uiso 1 1 calc R . . . .
C00F C 0.4770(5) 0.63009(12) 0.22004(8) 0.0178(4) Uani 1 1 d . . . . .
H00F H 0.370943 0.579203 0.204252 0.021 Uiso 1 1 calc R . . . .
C00G C 0.7653(5) 0.41666(11) 0.41329(9) 0.0179(4) Uani 1 1 d . . . . .
H00G H 0.871689 0.414797 0.371259 0.022 Uiso 1 1 calc R . . . .
C00H C 1.0156(5) 0.78956(11) 0.39692(8) 0.0165(4) Uani 1 1 d . . . . .
H00H H 1.092636 0.792765 0.441121 0.020 Uiso 1 1 calc R . . . .
C00I C 0.6763(5) 0.77383(12) 0.19995(9) 0.0185(4) Uani 1 1 d . . . . .
H00I H 0.704230 0.820816 0.170859 0.022 Uiso 1 1 calc R . . . .
C00J C 0.4819(5) 0.49886(11) 0.49663(9) 0.0174(4) Uani 1 1 d . . . . .
H00J H 0.387130 0.550943 0.512654 0.021 Uiso 1 1 calc R . . . .
C00K C 0.6071(5) 0.34956(12) 0.50812(9) 0.0212(4) Uani 1 1 d . . . . .
H00K H 0.595599 0.299053 0.533949 0.025 Uiso 1 1 calc R . . . .
C00L C 0.4741(5) 0.42471(12) 0.53412(9) 0.0200(4) Uani 1 1 d . . . . .
H00L H 0.378809 0.425464 0.577100 0.024 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
C007 N003 C008 124.75(14) . . ?
C007 N003 C00B 117.75(14) . . ?
C008 N003 C00B 117.47(13) . . ?
C00G N004 C00K 117.06(16) . . ?
C006 C005 C009 120.83(15) . . ?
C006 C005 C00A 119.54(16) . . ?
C009 C005 C00A 119.63(15) . . ?
C005 C006 C008 120.61(15) . . ?
C00H C006 C005 120.43(16) . . ?
C00H C006 C008 118.93(15) . . ?
O002 C007 N003 120.48(15) . . ?
O002 C007 C009 122.86(16) . . ?
N003 C007 C009 116.66(15) . . ?
O001 C008 N003 120.41(15) . . ?
O001 C008 C006 123.00(16) . . ?
N003 C008 C006 116.59(14) . . ?
C005 C009 C007 120.36(15) . . ?
C00F C009 C005 120.41(16) . . ?
C00F C009 C007 119.23(16) . . ?
C00C C00A C005 118.60(16) . . ?
C00I C00A C005 118.36(16) . . ?
C00I C00A C00C 123.04(16) . . ?
C00G C00B N003 119.05(15) . . ?
C00J C00B N003 121.51(15) . . ?
C00J C00B C00G 119.43(16) . . ?
C00A C00C H00C 119.7 . . ?
C00E C00C C00A 120.66(17) . . ?
C00E C00C H00C 119.7 . . ?
C00F C00D H00D 119.8 . . ?
C00I C00D H00D 119.8 . . ?
C00I C00D C00F 120.49(16) . . ?
C00C C00E H00E 119.6 . . ?
C00C C00E C00H 120.80(17) . . ?
C00H C00E H00E 119.6 . . ?
C009 C00F C00D 120.08(17) . . ?
C009 C00F H00F 120.0 . . ?
C00D C00F H00F 120.0 . . ?
N004 C00G C00B 123.28(17) . . ?
N004 C00G H00G 118.4 . . ?
C00B C00G H00G 118.4 . . ?
C006 C00H C00E 119.97(16) . . ?
C006 C00H H00H 120.0 . . ?
C00E C00H H00H 120.0 . . ?
C00A C00I H00I 119.5 . . ?
C00D C00I C00A 121.02(16) . . ?
C00D C00I H00I 119.5 . . ?
C00B C00J H00J 121.2 . . ?
C00B C00J C00L 117.64(16) . . ?
C00L C00J H00J 121.2 . . ?
N004 C00K H00K 118.3 . . ?
N004 C00K C00L 123.31(16) . . ?
C00L C00K H00K 118.3 . . ?
C00J C00L H00L 120.4 . . ?
C00K C00L C00J 119.26(16) . . ?
C00K C00L H00L 120.4 . . ?
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
O001 C008 1.213(2) . ?
O002 C007 1.213(2) . ?
N003 C007 1.411(2) . ?
N003 C008 1.414(2) . ?
N003 C00B 1.447(2) . ?
N004 C00G 1.336(2) . ?
N004 C00K 1.340(3) . ?
C005 C006 1.411(2) . ?
C005 C009 1.411(2) . ?
C005 C00A 1.421(2) . ?
C006 C008 1.477(2) . ?
C006 C00H 1.384(2) . ?
C007 C009 1.481(2) . ?
C009 C00F 1.381(2) . ?
C00A C00C 1.421(3) . ?
C00A C00I 1.417(2) . ?
C00B C00G 1.389(2) . ?
C00B C00J 1.383(2) . ?
C00C H00C 0.9500 . ?
C00C C00E 1.369(3) . ?
C00D H00D 0.9500 . ?
C00D C00F 1.405(3) . ?
C00D C00I 1.370(3) . ?
C00E H00E 0.9500 . ?
C00E C00H 1.405(2) . ?
C00F H00F 0.9500 . ?
C00G H00G 0.9500 . ?
C00H H00H 0.9500 . ?
C00I H00I 0.9500 . ?
C00J H00J 0.9500 . ?
C00J C00L 1.389(2) . ?
C00K H00K 0.9500 . ?
C00K C00L 1.387(3) . ?
C00L H00L 0.9500 . ?
