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_7227121
_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         'C55 H54 Co2 N2 O13'
_chemical_formula_sum            'C63 H72 Co2 N4 O15'
_chemical_formula_weight         1243.10
_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             2016-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_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                   32.094(2)
_cell_length_b                   9.8357(7)
_cell_length_c                   37.7628(16)
_cell_measurement_reflns_used    5877
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      58.72
_cell_measurement_theta_min      4.65
_cell_volume                     11920.5(12)
_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
;
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, 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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            52103
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.672
_diffrn_reflns_theta_min         3.615
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.950
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.355
_exptl_absorpt_correction_type   gaussian
_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)
Numerical absorption correction based on gaussian integration over a multifaceted crystal model
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5216
_exptl_crystal_recrystallization_method 'Solvothermal Reaction'
_exptl_crystal_size_max          0.3236
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.0544
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         11890
_refine_ls_number_restraints     758
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1346
_refine_ls_R_factor_gt           0.0836
_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^)+(0.1678P)^2^+0.8671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2382
_refine_ls_wR_factor_ref         0.2812
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6634
_reflns_number_total             11890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01965j2.cif
_cod_data_source_block           1-Co
_cod_depositor_comments
'Adding full bibliography for 7227120--7227122.cif.'
_cod_original_cell_volume        11920.5(13)
_cod_database_code               7227121
_nottingham_internal_coll_name   COADMW
_nottingham_internal_coll_number 12248
_nottingham_internal_coll_client ADM/MS
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time 25
_nottingham_internal_coll_frame_width 100
_nottingham_internal_coll_user   ADM
_nottingham_internal_coll_date   19/02/2013
_nottingham_internal_coll_location NOTT
_nottingham_internal_process_date 19/02/2013
_nottingham_internal_process_user ADM
_nottingham_internal_solution_date 19/02/2013
_nottingham_internal_solution_user ADM
_nottingham_internal_refinement_date 27/10/2015
_nottingham_internal_refinement_user ADM/pczspa
_nottingham_internal_validation_date 26/01/2016
_nottingham_internal_validation_user AJB
_olex2_refinement_description
;
1. 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
2. Shared sites
{O1C, O1B}
3. Uiso/Uaniso restraints and constraints
O12 \\sim O13 \\sim C78 \\sim C79 \\sim H79A \\sim H79C: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
O1B \\sim C2B \\sim C3B \\sim N4B \\sim C5B \\sim C6B \\sim O1C \\sim C2C \\sim
C3C \\sim N4C \\sim C5C \\sim C6C: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1C) = Uanis(O1B)
4. 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
5. Same fragment restrains
{O1A, C2A, C3A, N4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1B, C2B, C3B, N4B, C5B, C6B}
{O1A, C2A, C3A, N4A, C5A, C6A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1C, C2C, C3C, N4C, C5C, C6C}
6. 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)
7.a Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C2(H2A,H2B), C3(H3A,H3B)
7.b Me refined with riding coordinates:
 C79(H79A,H79B,H79C), 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)
7.c Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C15(H15), C18(H18), C19(H19), C21(H21), C22(H22), C32(H32),
 C35(H35), C38(H38), C39(H39), C41(H41), C42(H42), C52(H52), C55(H55), C58(H58),
  C59(H59), C61(H61), C62(H62)
7.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C36(H36A,H36B,H36C), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              9479
_shelx_fab_checksum              47157
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'