The effect of carboxylate position on the structure of a metal organic framework derived from cyclotriveratrylene
Martin, Adam D.; Easun, Timothy L.; Argent, Stephen P.; Lewis, William; Blake, Alexander J.; Schröder, Martin; CrystEngComm 19 (2017) 603–; doi:10.1039/C6CE01965J

data_7227120
_publ_section_title
;
 The effect of carboxylate position on the structure of a metal organic
 framework derived from cyclotriveratrylene
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              603
_journal_paper_doi               10.1039/C6CE01965J
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C54.36 H53.04 N2 O12.36 Zn2'
_chemical_formula_sum            'C59 H63 N3 O14 Zn2'
_chemical_formula_weight         1168.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-03-23 deposited with the CCDC.
2016-10-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.654(2)
_cell_length_b                   9.7728(7)
_cell_length_c                   37.310(2)
_cell_measurement_reflns_used    6053
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.0120
_cell_measurement_theta_min      2.1790
_cell_volume                     11541.8(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
;
 CrysAlisPro, Agilent Technologies, Version 1.171.36.28
 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb 1 2013,16:14:44)
;
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -60.00 115.00   1.00    1.00    --   30.00   0.00   0.00  175
  2  \w    -60.00  60.00   1.00    1.00    --   30.00 -50.00   0.00  120
  3  \w    -60.00  60.00   1.00    1.00    --   30.00 -50.00 120.00  120
  4  \w    -60.00  60.00   1.00    1.00    --   30.00 -50.00 240.00  120
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0162326000
_diffrn_orient_matrix_UB_12      0.0372023000
_diffrn_orient_matrix_UB_13      0.0074762000
_diffrn_orient_matrix_UB_21      -0.0116285000
_diffrn_orient_matrix_UB_22      -0.0080466000
_diffrn_orient_matrix_UB_23      -0.0154548000
_diffrn_orient_matrix_UB_31      -0.0086205000
_diffrn_orient_matrix_UB_32      -0.0593690000
_diffrn_orient_matrix_UB_33      0.0068137000
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_unetI/netI     0.1419
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            17110
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        20.191
_diffrn_reflns_theta_max         20.191
_diffrn_reflns_theta_min         2.179
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.16058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       plate
_exptl_crystal_F_000             4880
_exptl_crystal_recrystallization_method 'Solvothermal Reaction'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.143
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     609
_refine_ls_number_reflns         17110
_refine_ls_number_restraints     1020
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.2249
_refine_ls_R_factor_gt           0.1460
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3889
_refine_ls_wR_factor_ref         0.4154
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7317
_reflns_number_total             17110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01965j2.cif
_cod_data_source_block           1-Zn
_cod_depositor_comments
'Adding full bibliography for 7227120--7227122.cif.'
_cod_original_cell_volume        11542.0(14)
_cod_database_code               7227120
_nottingham_internal_coll_name   ZNADNM
_nottingham_internal_coll_number 12249
_nottingham_internal_coll_client ADM/MS
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time 1.00
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_date   28/04/2013
_nottingham_internal_coll_location DLS
_nottingham_internal_process_date 16/03/2016
_nottingham_internal_process_user pczspa
_nottingham_internal_solution_date 19/02/2013
_nottingham_internal_solution_user ADM
_nottingham_internal_refinement_date 17/03/2016
_nottingham_internal_refinement_user ADM/pczspa
_nottingham_internal_self_validation_date 27/10/2015
_nottingham_internal_self_validation_user pczspa
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_platon_squeeze_void_probe_radius 1.20
_chemical_oxdiff_formula         'C60 H45 O10 Zn3 N'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.710(3) 0.290(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{O1C, O1B}
4. Restrained distances
 O1A-C2A
 1.23 with sigma of 0.005
 C2A-N4A
 1.3 with sigma of 0.005
 O1A-N4A
 2.23 with sigma of 0.02
 C2A-C3A
 1.5 with sigma of 0.005
 N4A-C5A
 1.46 with sigma of 0.005
 N4A-C6A
 1.46 with sigma of 0.005
 C3A-N4A
 2.42 with sigma of 0.02
 C2A-C5A
 2.43 with sigma of 0.02
 C2A-C6A
 2.45 with sigma of 0.02
 C5A-C6A
 2.5 with sigma of 0.02
 O1B-C2B
 1.23 with sigma of 0.005
 C2B-N4B
 1.3 with sigma of 0.005
 O1B-N4B
 2.23 with sigma of 0.02
 O1C-C2C
 1.23 with sigma of 0.005
 C2C-N4C
 1.3 with sigma of 0.005
 O1C-N4C
 2.23 with sigma of 0.02
 C2B-C3B
 1.5 with sigma of 0.005
 N4B-C5B
 1.46 with sigma of 0.005
 N4B-C6B
 1.46 with sigma of 0.005
 C3B-N4B
 2.42 with sigma of 0.02
 C2B-C5B
 2.43 with sigma of 0.02
 C2B-C6B
 2.45 with sigma of 0.02
 C5B-C6B
 2.5 with sigma of 0.02
 C2C-C3C
 1.5 with sigma of 0.005
 N4C-C6C
 1.46 with sigma of 0.005
 C3C-N4C
 2.42 with sigma of 0.02
 C2C-C6C
 2.45 with sigma of 0.02
 O3D-O4D
 -2.1 with sigma of 0.02
 C2D-O3D = C2D-O4D
 1.25 with sigma of 0.02
 C1D-C2D
 1.5 with sigma of 0.1
 N4C-C5C
 1.46 with sigma of 0.005
 C2C-C5C
 2.43 with sigma of 0.02
 C5C-C6C
 2.5 with sigma of 0.02
 C16-C2 \\sim C31-C2 \\sim C36-C3 \\sim C3-C51 \\sim C56-C1 \\sim C11-C1
 with sigma of 0.02
 C31-C36 \\sim C11-C16 \\sim C51-C56
 with sigma of 0.02
 C12-C11 \\sim C15-C16 \\sim C32-C31 \\sim C35-C36 \\sim C52-C51 \\sim C55-C56
 with sigma of 0.02
 C21-C13 \\sim C61-C53 \\sim C41-C33
 with sigma of 0.02
 C47-C44 \\sim C27-C24 \\sim C67-C64
 with sigma of 0.02
 O37-C34 \\sim O17-C14 \\sim O57-C54
 with sigma of 0.02
 C16-C31 \\sim C36-C51 \\sim C56-C11
 with sigma of 0.02
 O57-C58 \\sim O17-C18 \\sim O37-C38
 with sigma of 0.02
 C58-C54 \\sim C18-C15 \\sim C34-C38
 with sigma of 0.02
 Zn2-O4D \\sim Zn2-O3D
 with sigma of 0.05
 C1D-O3D \\sim C1D-O4D
 with sigma of 0.02
5. Restrained planarity
 O1A, C2A, C3A, N4A, C5A, C6A
 with sigma of 0.1
 O1B, C2B, C3B, N4B, C5B, C6B
 with sigma of 0.1
 O4D, O3D, C2D, C1D
 with sigma of 0.1
 O1C, C2C, C3C, N4C, C5C, C6C
 with sigma of 0.1
6. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uiso(O1C) = Uiso(O1B)
7. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
8. Others
 Sof(O1C)=Sof(C2C)=Sof(C3C)=Sof(H3Ca)=Sof(H3Cb)=Sof(H3Cc)=Sof(N4C)=Sof(C5C)=
 Sof(H5Ca)=Sof(H5Cb)=Sof(H5Cc)=Sof(C6C)=Sof(H6Ca)=Sof(H6Cb)=Sof(H6Cc)=1-FVAR(1)
 Sof(O1B)=Sof(C2B)=Sof(C3B)=Sof(H3Ba)=Sof(H3Bb)=Sof(H3Bc)=Sof(N4B)=Sof(C5B)=
 Sof(H5Ba)=Sof(H5Bb)=Sof(H5Bc)=Sof(C6B)=Sof(H6Ba)=Sof(H6Bb)=Sof(H6Bc)=FVAR(1)
 Uiso(O1B)=Uiso(C2B)=Uiso(C3B)=Uiso(N4B)=Uiso(C5B)=Uiso(C6B)=Uiso(O1C)=FVAR(2)
 Uiso(C2C)=Uiso(C3C)=Uiso(N4C)=Uiso(C5C)=Uiso(C6C)=FVAR(3)
 Sof(O4D)=Sof(O3D)=Sof(C2D)=Sof(C1D)=Sof(H1Da)=Sof(H1Db)=Sof(H1Dc)=FVAR(4)
 Fixed Uiso: O4D(0.2) O3D(0.2) C2D(0.2) C1D(0.2)
9.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C3(H3a,H3b), C2(H2a,H2b)
9.b Me refined with riding coordinates:
 C58(H58a,H58b,H58c), C38(H38a,H38b,H38c), C18(H18a,H18b,H18c), C3A(H3Aa,H3Ab,
 H3Ac), C5A(H5Aa,H5Ab,H5Ac), C6A(H6Aa,H6Ab,H6Ac), C3B(H3Ba,H3Bb,H3Bc), C5B(H5Ba,
 H5Bb,H5Bc), C6B(H6Ba,H6Bb,H6Bc), C3C(H3Ca,H3Cb,H3Cc), C5C(H5Ca,H5Cb,H5Cc),
 C6C(H6Ca,H6Cb,H6Cc), C1D(H1Da,H1Db,H1Dc)
9.c Aromatic/amide H refined with riding coordinates:
 C52(H52), C55(H55), C62(H62), C63(H63), C65(H65), C66(H66), C32(H32),
 C35(H35), C42(H42), C43(H43), C45(H45), C46(H46), C12(H12), C15(H15), C22(H22),
  C23(H23), C25(H25), C26(H26)
;
_shelx_res_checksum              17779
_shelx_fab_checksum              81531
_shelx_shelxl_version_number     2014/7
_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 3.409
_oxdiff_exptl_absorpt_empirical_full_min 0.480
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by 178.9382\% 
 around [-0.03 0.03 1.00] (reciprocal) or [-0.04 0.35 0.94] (direct)
;