2D networks of metallo-capsules and other coordination polymers from a hexapodal ligand
Thorp-Greenwood, Flora L.; Berry, Gilberte Therese; Boyadjieva, Sophia S.; Oldknow, Samuel; Hardie, Michaele J.; CrystEngComm 20 (2018) 3960–; doi:10.1039/C8CE00806J

data_7231030
_publ_section_title
;
 2D networks of metallo-capsules and other coordination polymers from a
 hexapodal ligand
;
_journal_issue                   28
_journal_name_full               CrystEngComm
_journal_page_first              3960
_journal_paper_doi               10.1039/C8CE00806J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C69 H40 Cu2 F9 N7 O20'
_chemical_formula_sum            'C69 H40 Cu2 F9 N7 O20'
_chemical_formula_weight         1585.16
_chemical_name_common
;
[hexakis(isonicotinoyl)cyclotricatechylene]
tris(trifluoroacetate)(isoniconinate)dicopper(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-08-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-02-09 deposited with the CCDC.
2018-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                103.319(6)
_cell_angle_beta                 109.243(6)
_cell_angle_gamma                103.091(5)
_cell_formula_units_Z            2
_cell_length_a                   18.1806(11)
_cell_length_b                   18.4809(11)
_cell_length_c                   19.4599(13)
_cell_measurement_reflns_used    4116
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      49.4030
_cell_measurement_theta_min      3.8310
_cell_volume                     5672.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_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     21.00  61.00   1.00    2.00    --    0.00  57.00  30.00   40
  2  \w     31.00 133.00   1.00    8.00    --   59.61  19.00 150.00  102
  3  \w     55.00  80.00   1.00    8.00    --   59.61 -65.00  88.14   25
  4  \w     53.00  87.00   1.00    8.00    --   59.61 -65.00 144.54   34
  5  \w     50.00  87.00   1.00    8.00    --   59.61 -65.00  36.91   37
  6  \w     60.00  87.00   1.00    8.00    --   59.61 -65.00 -66.23   27
  7  \w     53.00  81.00   1.00    8.00    --   59.61 -64.00 -86.31   28
  8  \w     52.00  87.00   1.00    8.00    --   59.61 -64.00-121.27   35
  9  \w     52.00  82.00   1.00    8.00    --   59.61 -65.00-170.05   30
 10  \w     51.00  79.00   1.00    8.00    --   59.61 -65.00-150.86   28
 11  \w     27.00  87.00   1.00    8.00    --   59.61 -65.00  -6.78   60
 12  \w     17.00  77.00   1.00    8.00    --   59.61 -65.00 127.28   60
 13  \w    -17.00  90.00   1.00    8.00    --   59.61 -19.00 -60.00  107
 14  \w     72.00 124.00   1.00    8.00    --   59.61  65.00-177.21   52
 15  \w     32.00  59.00   1.00    8.00    --   59.61  65.00-177.21   27
 16  \w     -7.00  39.00   1.00    8.00    --   59.61 -64.00 -86.31   46
 17  \w     -9.00  29.00   1.00    8.00    --   59.61 -64.00-121.27   38
 18  \w    -59.00 -32.00   1.00    2.00    --    0.00 -57.00-180.00   27
 19  \w    -25.00  18.00   1.00    2.00    --    0.00  57.00  30.00   43
 20  \w    -65.00  24.00   1.00    2.00    --    0.00 -57.00-120.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0409991000
_diffrn_orient_matrix_UB_12      -0.0618341000
_diffrn_orient_matrix_UB_13      -0.0191662000
_diffrn_orient_matrix_UB_21      -0.0701087000
_diffrn_orient_matrix_UB_22      -0.0386218000
_diffrn_orient_matrix_UB_23      -0.0812454000
_diffrn_orient_matrix_UB_31      0.0493770000
_diffrn_orient_matrix_UB_32      0.0539912000
_diffrn_orient_matrix_UB_33      -0.0305289000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0778
_diffrn_reflns_av_unetI/netI     0.1295
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27829
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        51.417
_diffrn_reflns_theta_max         51.417
_diffrn_reflns_theta_min         2.978
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.928
_exptl_crystal_description       block
_exptl_crystal_F_000             1604
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
TITL tbl1cutfa_a.res in P-1
CELL   18.1806   18.4809   19.4599    103.32    109.24    103.09
SPGR P-1
C101 0.327 0.207 0.181 !      11.90 eA-3
C102 0.510 0.565 0.279 !       9.83 eA-3
C103 0.529 0.072 0.144 !       8.14 eA-3
C104 0.265 0.716 0.044 !       7.13 eA-3
C105 0.776 0.280 0.293 !       5.82 eA-3
C106 0.383 0.186 0.159 !       5.41 eA-3
C107 0.379 0.947 0.486 !       4.80 eA-3
C108 0.504 0.495 0.214 !       4.62 eA-3
C109 0.735 0.816 0.420 !       4.06 eA-3
C110 0.560 0.021 0.106 !       3.85 eA-3
C111 0.780 0.748 0.238 !       3.83 eA-3
C112 0.487 0.518 0.345 !       3.58 eA-3
C113 0.821 0.285 0.022 !       3.50 eA-3
C114 0.232 0.146 0.108 !       3.30 eA-3
C115 0.023 0.654 0.203 !       3.21 eA-3
C116 0.393 0.969 0.403 !       3.11 eA-3
C117 0.877 0.824 0.292 !       3.05 eA-3
C118 0.561 0.139 0.074 !       3.02 eA-3
C119 0.012 0.661 0.127 !       2.99 eA-3
C120 0.635 0.248 0.067 !       2.97 eA-3
C121 0.731 0.029 0.140 !       2.90 eA-3
C122 0.801 0.192 0.280 !       2.87 eA-3
C123 0.895 0.097 0.452 !       2.87 eA-3
C124 0.328 0.984 0.425 !       2.84 eA-3
C125 0.863 0.360 0.339 !       2.81 eA-3
C126 0.358 0.919 0.390 !       2.76 eA-3
C127 0.799 1.007 0.265 !       2.75 eA-3
C128 0.867 0.792 0.327 !       2.66 eA-3
C129 0.328 0.299 0.200 !       2.63 eA-3
C130 0.453 0.032 0.112 !       2.62 eA-3
C131 0.126 0.658 0.233 !       2.58 eA-3
C132 0.766 0.059 0.056 !       2.57 eA-3
C133 0.112 0.671 0.019 !       2.57 eA-3
C134 0.596 0.592 0.330 !       2.51 eA-3
C135 0.155 0.103 0.411 !       2.50 eA-3
C136 0.747 0.269 0.207 !       2.48 eA-3
C137 0.329 0.093 0.411 !       2.47 eA-3
C138 0.318 0.958 0.372 !       2.40 eA-3
C139 0.113 0.095 0.372 !       2.34 eA-3
C140 0.666 0.309-0.004 !       2.33 eA-3
C141 0.581 0.952 0.490 !       2.30 eA-3
C142 0.486 0.481 0.280 !       2.29 eA-3
C143 0.807 0.194 0.109 !       2.28 eA-3
C144 0.805 0.750 0.319 !       2.27 eA-3
C145 0.126 0.745 0.214 !       2.26 eA-3
C146 0.965 0.623 0.112 !       2.22 eA-3
C147 0.826 0.084 0.407 !       2.14 eA-3
C148 0.358 0.070 0.436 !       2.09 eA-3
C149 0.170 0.099 0.346 !       2.08 eA-3
C150 0.799 0.820 0.232 !       2.05 eA-3
C151 0.357 0.747 0.027 !       1.96 eA-3
C152 0.277 0.622 0.020 !       1.95 eA-3
C153 0.991 0.451 0.073 !       1.94 eA-3
C154 0.797 0.258 0.060 !       1.92 eA-3
C155 0.926 0.552 0.060 !       1.85 eA-3
C156 0.092 0.112 0.454 !       1.85 eA-3
C157 0.784 0.794 0.315 !       1.84 eA-3
C158 0.292 0.776 0.029 !       1.81 eA-3
C159 0.325 0.939 0.348 !       1.80 eA-3
Q160 0.892 0.622 0.473 !       1.77 eA-3
C161 0.911 0.581 0.033 !       1.74 eA-3
C162 0.715 0.285 0.061 !       1.72 eA-3
C163 0.939 0.531 0.024 !       1.71 eA-3
Q164 0.013 0.689 0.277 !       1.70 eA-3
C165 0.968 0.112 0.419 !       1.69 eA-3
C166 0.960 0.094 0.436 !       1.68 eA-3
Q167 0.952 0.647 0.462 !       1.66 eA-3
C168 0.629 0.606 0.376 !       1.66 eA-3
C169 0.968 0.357 0.035 !       1.66 eA-3
C170 0.892 0.851 0.359 !       1.63 eA-3
C171 0.954 0.116 0.504 !       1.63 eA-3
C172 0.074 0.982 0.343 !       1.61 eA-3
C173 0.824 0.210 0.182 !       1.59 eA-3
C174 0.704 0.036 0.506 !       1.58 eA-3
Q175 0.319 0.880 0.437 !       1.57 eA-3
C176 0.877 0.909 0.303 !       1.55 eA-3
C177 0.757 0.189 0.236 !       1.55 eA-3
C178 0.815 0.048 0.328 !       1.53 eA-3
C179 0.940 0.016 0.445 !       1.52 eA-3
C180 0.921 0.454 0.036 !       1.51 eA-3
C181 0.268 0.912 0.353 !       1.50 eA-3
C182 0.653 0.188-0.001 !       1.50 eA-3
C183 0.962 0.781 0.283 !       1.48 eA-3
C184 0.828 0.076 0.297 !       1.47 eA-3
Q185 0.846 0.579 0.393 !       1.46 eA-3
C186 0.015 0.620 0.077 !       1.46 eA-3
C187 0.448 0.036 0.480 !       1.44 eA-3
C188 0.280 0.929 0.429 !       1.44 eA-3
C189 0.396 0.027 0.442 !       1.43 eA-3
C190 0.283 0.151 0.499 !       1.42 eA-3
Q191 0.896 0.139 0.499 !       1.41 eA-3
C192 0.997 0.587 0.148 !       1.41 eA-3
Q193 0.258 0.901 0.467 !       1.40 eA-3
Q194 0.934 0.652 0.233 !       1.40 eA-3
C195 0.372 0.251 0.237 !       1.39 eA-3
C196 0.487 0.918 0.085 !       1.38 eA-3
C197 0.992 0.529 0.082 !       1.38 eA-3
C198 0.971 0.434 0.011 !       1.38 eA-3
Q199 0.905 0.623 0.256 !       1.37 eA-3
;
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         11988
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1792
_refine_ls_R_factor_gt           0.1249
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1826P)^2^+38.2928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3474
_refine_ls_wR_factor_ref         0.3868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6609
_reflns_number_total             11988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00806j2.cif
_cod_data_source_block           cutfa_sq
_cod_depositor_comments
'Adding full bibliography for 7231022--7231030.cif.'
_cod_database_code               7231030
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.932
_reflns_odcompleteness_completeness 98.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C64-C65
 1.45 with sigma of 0.02
 C68-C70
 1.45 with sigma of 0.02
 O15-C68
 1.35 with sigma of 0.02
3. Restrained planarity
 O16, C64, C65, O17
 with sigma of 0.1
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12), C16(H16), C19(H19), C24(H24), C25(H25),
 C26(H26), C27(H27), C30(H30), C31(H31), C32(H32), C33(H33), C36(H36), C37(H37),
  C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C45(H45), C48(H48),
 C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56), C57(H57), C60(H60),
  C61(H61), C62(H62), C63(H63)
;
_platon_squeeze_void_probe_radius 1.20
_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 1.257
_oxdiff_exptl_absorpt_empirical_full_min 0.904