#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:11:04 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185179 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/57/7225728.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_7225728
loop_
_publ_author_name
'Keenan, Luke L.'
'Hamzah, Harina Amer'
'Mahon, Mary F.'
'Warren, Mark R.'
'Burrows, Andrew D.'
_publ_section_title
;
 Secondary amine-functionalised metal--organic frameworks: direct
 syntheses versus tandem post-synthetic modifications
;
_journal_issue                   30
_journal_name_full               CrystEngComm
_journal_page_first              5710
_journal_paper_doi               10.1039/C6CE01270A
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         '0.25(C108 N12 O52 Zn16)'
_chemical_formula_sum            'C77.1 H83.4 N3 O13 Zn4'
_chemical_formula_weight         1521.54
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-29 deposited with the CCDC.
2016-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.77025(14)
_cell_length_b                   25.77025(14)
_cell_length_c                   25.77025(14)
_cell_measurement_reflns_used    8958
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      28.7600
_cell_measurement_theta_min      2.5240
_cell_volume                     17114.17(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      250.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
;
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26286
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         27.719
_diffrn_reflns_theta_min         2.541
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_description       block
_exptl_crystal_F_000             6328
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.704
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         1163
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0382
_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)+(0.0901P)²+5.2817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1004
_reflns_number_total             1163
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01270a2.cif
_cod_data_source_block           dlk30_sq
_cod_depositor_comments
'Adding full bibliography for 7225726--7225730.cif.'
_cod_original_cell_volume        17114.2(3)
_cod_original_formula_sum        'C77.10 H83.40 N3 O13 Zn4'
_cod_database_code               7225728
_shelxl_version_number           2014-3
_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   0.929
_shelx_estimated_absorpt_t_min   0.882
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.03 and sigma for
terminal atoms of 0.06
2. Others
 Fixed Sof: N1(0.125) C4(0.125)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, z+1/2, -y+1/2'
'-x, y+1/2, z+1/2'
'-x, -z+1/2, y+1/2'
'-z, -y+1/2, x+1/2'
'x, -y+1/2, z+1/2'
'z, -y+1/2, -x+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-z, y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, z, -y+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -z, y+1/2'
'-z+1/2, -y, x+1/2'
'x+1/2, -y, z+1/2'
'z+1/2, -y, -x+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, z+1/2, -y'
'-x+1/2, y+1/2, z'
'-x+1/2, -z+1/2, y'
'-z+1/2, -y+1/2, x'
'x+1/2, -y+1/2, z'
'z+1/2, -y+1/2, -x'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-z+1/2, y+1/2, -x'
'z+1/2, y+1/2, x'
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
Zn1 Zn 0.29332(2) 0.20668(2) 0.20668(2) 0.0347(2) Uani 1 6 d S T P
O1 O 0.2500 0.2500 0.2500 0.0318(8) Uani 1 24 d S T P
O2 O 0.36598(7) 0.21938(6) 0.21938(6) 0.0636(5) Uani 1 2 d S T P
N1 N 0.4497(5) 0.3192(4) 0.3192(4) 0.149(7) Uani 0.25 2 d S TU P
C1 C 0.38859(11) 0.2500 0.2500 0.0524(8) Uani 1 4 d S T P
C2 C 0.44609(12) 0.2500 0.2500 0.0606(9) Uani 1 4 d S T P
C3 C 0.47326(12) 0.28236(10) 0.28236(10) 0.0922(13) Uani 1 2 d S T P
C4 C 0.4764(9) 0.3540(6) 0.3540(6) 0.196(11) Uani 0.25 2 d S TU P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3260 1.3880 '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
Zn1 Zn1 Zn1 60.0 148 75
Zn1 Zn1 Zn1 60.0 122 75
Zn1 Zn1 Zn1 60.0 148 122
O1 Zn1 Zn1 35.3 . 148
O1 Zn1 Zn1 35.3 . 75
O1 Zn1 Zn1 35.3 . 122
O2 Zn1 Zn1 76.11(6) . 148
O2 Zn1 Zn1 124.50(5) 63 122
O2 Zn1 Zn1 124.50(5) . 75
O2 Zn1 Zn1 124.50(5) 63 148
O2 Zn1 Zn1 76.11(6) 88 122
O2 Zn1 Zn1 124.50(5) 88 148
O2 Zn1 Zn1 124.50(5) 88 75
O2 Zn1 Zn1 124.50(5) . 122
O2 Zn1 Zn1 76.11(6) 63 75
O2 Zn1 O1 111.37(6) . .
O2 Zn1 O1 111.37(6) 63 .
O2 Zn1 O1 111.37(6) 88 .
O2 Zn1 O2 107.50(7) . 63
O2 Zn1 O2 107.51(7) 63 88
O2 Zn1 O2 107.50(7) . 88
Zn1 O1 Zn1 109.5 148 122
Zn1 O1 Zn1 109.5 122 .
Zn1 O1 Zn1 109.5 75 .
Zn1 O1 Zn1 109.5 75 122
Zn1 O1 Zn1 109.5 148 .
Zn1 O1 Zn1 109.5 148 75
C1 O2 Zn1 131.45(17) . .
C4 N1 C3 127.2(12) . .
O2 C1 O2 124.9(3) 30 .
O2 C1 C2 117.56(14) . .
O2 C1 C2 117.57(14) 30 .
C3 C2 C1 120.69(17) 30 .
C3 C2 C1 120.69(17) . .
C3 C2 C3 118.6(3) . 30
C2 C3 N1 125.0(6) . .
C2 C3 C3 120.70(17) . 102_655
C3 C3 N1 114.3(5) 102_655 .
C4 C4 N1 118.5(10) 102_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 Zn1 3.1578(6) 122
Zn1 Zn1 3.1578(6) 75
Zn1 Zn1 3.1578(6) 148
Zn1 O1 1.9337(4) .
Zn1 O2 1.9290(17) 63
Zn1 O2 1.9290(17) 88
Zn1 O2 1.9289(17) .
O1 Zn1 1.9337(4) 148
O1 Zn1 1.9337(4) 75
O1 Zn1 1.9337(4) 122
O2 C1 1.259(2) .
N1 C3 1.474(13) .
N1 C4 1.44(3) .
C1 O2 1.259(2) 30
C1 C2 1.482(4) .
C2 C3 1.372(4) .
C2 C3 1.372(4) 30
C3 C3 1.378(6) 102_655
C4 C4 1.22(5) 102_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Zn1 O2 C1 O2 0.000(0) . 30
Zn1 O2 C1 C2 180.000(0) . .
O2 C1 C2 C3 0.000(0) . 30
O2 C1 C2 C3 180.000(0) 30 30
O2 C1 C2 C3 0.000(0) 30 .
O2 C1 C2 C3 180.000(0) . .
C1 C2 C3 N1 0.000(1) . .
C1 C2 C3 C3 180.000(0) . 102_655
C3 N1 C4 C4 0.000(4) . 102_655
C3 C2 C3 N1 180.000(1) 30 .
C3 C2 C3 C3 0.000(0) 30 102_655
C4 N1 C3 C2 180.000(1) . .
C4 N1 C3 C3 0.000(1) . 102_655
