#------------------------------------------------------------------------------
#$Date: 2019-10-28 01:57:09 +0200 (Mon, 28 Oct 2019) $
#$Revision: 219558 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/72/4127287.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_4127287
loop_
_publ_author_name
'Yu, Mei-Hui'
'Space, Brian'
'Franz, Douglas'
'Zhou, Wei'
'He, Chaohui'
'Li, Libo'
'Krishna, Rajamani'
'Chang, Ze'
'Li, Wei'
'Hu, Tong-Liang'
'Bu, Xian-He'
_publ_section_title
;
 Enhanced Gas Uptake in a Microporous Metal-Organic Framework via a
 Sorbate Induced-Fit Mechanism.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b07807
_journal_year                    2019
_chemical_formula_moiety         'C13 H6 Cu F N O4, 0.13(N2)'
_chemical_formula_sum            'C52 H24 Cu4 F4 N5 O16'
_chemical_formula_weight         1304.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.488(2)
_cell_length_b                   10.412(2)
_cell_length_c                   15.057(3)
_cell_measurement_reflns_used    3807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.173
_cell_measurement_theta_min      2.821
_cell_volume                     1571.3(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.925
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       14
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       14
_diffrn_reflns_limit_l_max       -20
_diffrn_reflns_limit_l_min       19
_diffrn_reflns_number            3807
_diffrn_reflns_point_group_measured_fraction_full 0.925
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.173
_diffrn_reflns_theta_min         2.821
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             651
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.008
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3807
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0756
_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)+(0.1231P)²+4.5674P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2463
_refine_ls_wR_factor_ref         0.2517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3340
_reflns_number_total             3807
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            NKU-FlexMOF-1a-N2-a.cif
_cod_data_source_block           NKU-FlexMOF-1a-N2-a
_cod_database_code               4127287
_shelx_shelxl_version_number     2014/7
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N13-N14
 1.18 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N13 \\sim N14: within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.05
Uanis(N13) \\sim Ueq, Uanis(N14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.05
4. Others
 Fixed Sof: N13(0.125) N14(0.125)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C5(H5), C6(H6), C14(H14), C13(H13), C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
O4 O 0.5298(3) 0.1737(4) 0.4304(3) 0.0526(9) Uani 1 1 d . . .
Cu1 Cu 0.59182(6) 0.58948(6) 0.01064(4) 0.0462(3) Uani 1 1 d . . .
C1 C 0.6315(5) 0.4162(5) 0.1569(4) 0.0494(12) Uani 1 1 d . . .
C2 C 0.7058(5) 0.3584(5) 0.2491(4) 0.0488(11) Uani 1 1 d . . .
C9 C 1.1144(5) 0.4662(6) 0.4109(4) 0.0547(12) Uani 1 1 d . . .
H9 H 1.0603 0.5378 0.3913 0.066 Uiso 1 1 calc R . .
C4 C 0.9139(5) 0.3215(6) 0.3684(4) 0.0506(11) Uani 1 1 d . . .
C5 C 0.8493(5) 0.2370(6) 0.4111(4) 0.0513(12) Uani 1 1 d . . .
H5 H 0.8978 0.1926 0.4638 0.062 Uiso 1 1 calc R . .
C6 C 0.8415(5) 0.3820(6) 0.2870(4) 0.0507(12) Uani 1 1 d . . .
H6 H 0.8843 0.4388 0.2575 0.061 Uiso 1 1 calc R . .
C10 C 1.0604(5) 0.3445(6) 0.4070(4) 0.0507(12) Uani 1 1 d . . .
C7 C 0.7120(5) 0.2175(6) 0.3759(4) 0.0498(11) Uani 1 1 d . . .
F1 F 1.3075(4) 0.5954(3) 0.4496(3) 0.0699(11) Uani 1 1 d . . .
C14 C 1.1475(5) 0.2418(6) 0.4359(4) 0.0492(11) Uani 1 1 d . . .
H14 H 1.1121 0.1594 0.4321 0.059 Uiso 1 1 calc R . .
C13 C 1.3316(5) 0.3743(6) 0.4736(4) 0.0538(12) Uani 1 1 d . . .
H13 H 1.4234 0.3855 0.4966 0.065 Uiso 1 1 calc R . .
C12 C 1.2512(5) 0.4781(6) 0.4450(5) 0.0567(13) Uani 1 1 d . . .
O3 O 0.5228(4) 0.3631(4) 0.1140(3) 0.0530(9) Uani 1 1 d . . .
O1 O 0.6839(4) 0.5104(4) 0.1303(3) 0.0540(9) Uani 1 1 d . . .
N3 N 1.2795(4) 0.2559(5) 0.4687(3) 0.0491(10) Uani 1 1 d . . .
O2 O 0.6943(4) 0.0269(4) 0.4554(3) 0.0562(9) Uani 1 1 d . . .
C21 C 0.6402(5) 0.1322(6) 0.4244(4) 0.0508(12) Uani 1 1 d . . .
C20 C 0.6416(5) 0.2781(6) 0.2939(4) 0.0509(12) Uani 1 1 d . . .
H20 H 0.5504 0.2642 0.2694 0.061 Uiso 1 1 calc R . .
N13 N 0.869(6) 0.783(7) 0.328(4) 0.103(17) Uani 0.125 1 d D U P
N14 N 0.759(6) 0.789(7) 0.279(4) 0.098(16) Uani 0.125 1 d D U P
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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
C21 O4 Cu1 127.7(4) . 2_645
O4 Cu1 Cu1 79.71(12) 2_655 3_665
O4 Cu1 O3 91.37(17) 2_655 3_665
O4 Cu1 N3 92.20(17) 2_655 2_755
O3 Cu1 Cu1 80.92(12) 3_665 3_665
O3 Cu1 N3 96.64(17) 3_665 2_755
O1 Cu1 O4 88.93(17) . 2_655
O1 Cu1 Cu1 87.66(12) . 3_665
O1 Cu1 O3 168.34(17) . 3_665
O1 Cu1 N3 95.00(17) . 2_755
O1 Cu1 O2 87.00(18) . 4_565
N3 Cu1 Cu1 171.45(13) 2_755 3_665
O2 Cu1 O4 168.21(17) 4_565 2_655
O2 Cu1 Cu1 89.07(12) 4_565 3_665
O2 Cu1 O3 90.40(18) 4_565 3_665
O2 Cu1 N3 99.17(17) 4_565 2_755
O3 C1 C2 116.2(5) . .
O1 C1 C2 117.0(5) . .
O1 C1 O3 126.8(5) . .
C6 C2 C1 119.9(5) . .
C20 C2 C1 120.2(5) . .
C20 C2 C6 119.9(5) . .
C12 C9 C10 117.8(5) . .
C5 C4 C6 119.0(5) . .
C5 C4 C10 120.7(5) . .
C6 C4 C10 120.2(5) . .
C4 C5 C7 120.6(5) . .
C4 C6 C2 120.6(5) . .
C9 C10 C4 121.7(5) . .
C9 C10 C14 117.9(5) . .
C14 C10 C4 120.3(5) . .
C5 C7 C21 121.1(5) . .
C20 C7 C5 119.3(5) . .
C20 C7 C21 119.6(5) . .
N3 C14 C10 123.1(5) . .
N3 C13 C12 120.6(5) . .
F1 C12 C9 119.4(5) . .
F1 C12 C13 118.8(5) . .
C13 C12 C9 121.8(5) . .
C1 O3 Cu1 125.7(4) . 3_665
C1 O1 Cu1 118.8(3) . .
C14 N3 Cu1 120.0(4) . 2_745
C14 N3 C13 118.9(5) . .
C13 N3 Cu1 120.1(3) . 2_745
C21 O2 Cu1 116.9(3) . 4_566
O4 C21 C7 116.0(5) . .
O2 C21 O4 126.4(5) . .
O2 C21 C7 117.6(5) . .
C2 C20 C7 120.4(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O4 Cu1 1.963(4) 2_645
O4 C21 1.263(6) .
Cu1 O4 1.963(4) 2_655
Cu1 Cu1 2.6306(13) 3_665
Cu1 O3 1.971(4) 3_665
Cu1 O1 1.958(4) .
Cu1 N3 2.161(5) 2_755
Cu1 O2 1.960(4) 4_565
C1 C2 1.503(7) .
C1 O3 1.261(6) .
C1 O1 1.246(7) .
C2 C6 1.390(7) .
C2 C20 1.370(8) .
C9 C10 1.382(8) .
C9 C12 1.380(7) .
C4 C5 1.379(8) .
C4 C6 1.388(8) .
C4 C10 1.493(7) .
C5 C7 1.395(7) .
C10 C14 1.391(8) .
C7 C21 1.487(8) .
C7 C20 1.390(7) .
F1 C12 1.350(7) .
C14 N3 1.334(6) .
C13 C12 1.360(8) .
C13 N3 1.342(8) .
O3 Cu1 1.971(4) 3_665
N3 Cu1 2.161(5) 2_745
O2 Cu1 1.960(4) 4_566
O2 C21 1.260(7) .
N13 N14 1.180(10) .
