p-Xylylenediamine derived ligands as flexible connectors in the design of porous coordination polymers
Emerson, Adrian J.; Knowles, Gregory P.; Chaffee, Alan L.; Batten, Stuart R.; Turner, David R.; CrystEngComm 21 (2019) 3074–; doi:10.1039/C9CE00371A

data_7232625
_publ_section_title
;
 p-Xylylenediamine derived ligands as flexible connectors in the design of
 porous coordination polymers
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3074
_journal_paper_doi               10.1039/C9CE00371A
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C86 H86 Co4 N6 O22, C3 H7 N O'
_chemical_formula_sum            'C89 H93 Co4 N7 O23'
_chemical_formula_weight         1864.42
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-05 deposited with the CCDC.    2019-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                72.50(3)
_cell_angle_beta                 88.77(3)
_cell_angle_gamma                85.34(3)
_cell_formula_units_Z            2
_cell_length_a                   14.101(3)
_cell_length_b                   16.998(3)
_cell_length_c                   21.305(4)
_cell_measurement_reflns_used    26694
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.101
_cell_measurement_theta_min      1.002
_cell_volume                     4854.1(18)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1566
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            116086
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.101
_diffrn_reflns_theta_min         1.002
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_recrystallization_method 'From reaction mixture'
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
TITL 5.res in P-1
CELL   14.1010   16.9980   21.3050     72.50     88.77     85.34
SPGR P-1
Q101 1.000 1.000 0.500 !       5.71 eA-3
C102 0.887 0.328 0.300 !       4.00 eA-3
Q103 1.000 1.000 0.000 !       3.88 eA-3
C104 0.121 0.427 0.464 !       3.88 eA-3
C105 0.985 0.785 0.272 !       3.42 eA-3
C106 0.845 0.296 0.207 !       3.36 eA-3
C107 0.956 0.690 0.281 !       3.29 eA-3
C108 0.031 0.627 0.307 !       3.15 eA-3
C109 0.107 0.621 0.326 !       3.05 eA-3
C110 0.237 0.507 0.442 !       2.95 eA-3
C111 0.925 0.737 0.284 !       2.74 eA-3
C112 0.934 0.412 0.246 !       2.73 eA-3
C113 0.137 0.406 0.399 !       2.54 eA-3
Q114 0.876 0.058 0.125 !       2.50 eA-3
C115 0.848 0.302 0.246 !       2.48 eA-3
C116 0.171 0.467 0.486 !       2.45 eA-3
C117 0.890 0.289 0.381 !       2.44 eA-3
C118 0.939 0.639 0.487 !       2.38 eA-3
C119 0.812 0.321 0.129 !       2.16 eA-3
Q120 0.890 0.924 0.387 !       1.96 eA-3
C121 0.861 0.696 0.267 !       1.94 eA-3
C122 0.831 0.244 0.319 !       1.88 eA-3
Q123 0.846 0.946 0.385 !       1.83 eA-3
C124 0.863 0.515 0.462 !       1.59 eA-3
C125 0.863 0.614 0.284 !       1.35 eA-3
C126 0.892 0.453 0.380 !       1.31 eA-3
Q127 0.063 0.046 0.408 !       1.28 eA-3
Q128 0.864 0.984 0.467 !       1.21 eA-3
C129 0.891 0.447 0.330 !       1.20 eA-3
C130 0.172 0.462 0.436 !       1.20 eA-3
C131 0.889 0.421 0.299 !       1.14 eA-3
C132 0.047 0.677 0.286 !       1.09 eA-3
C133 0.113 0.556 0.363 !       1.05 eA-3
Q134 0.970 0.033 0.325 !       1.03 eA-3
Q135 0.889 0.086 0.004 !       0.98 eA-3
C136 0.937 0.797 0.231 !       0.96 eA-3
Q137 0.031 0.923 0.098 !       0.94 eA-3
Q138 0.731 0.128 0.386 !       0.94 eA-3
Q139 0.052 0.692 0.235 !       0.93 eA-3
C140 0.985 0.392 0.488 !       0.91 eA-3
Q141 0.984 0.979 0.172 !       0.88 eA-3
C142 0.783 0.349 0.172 !       0.86 eA-3
Q143 0.901 0.051 0.428 !       0.86 eA-3
Q144 0.736 0.107 0.001 !       0.86 eA-3
C145 0.913 0.773 0.235 !       0.85 eA-3
Q146 0.893 0.129 0.074 !       0.84 eA-3
C147 0.081 0.501 0.377 !       0.83 eA-3
Q148 0.747 0.078 0.407 !       0.83 eA-3
C149 0.904 0.674 0.419 !       0.83 eA-3
C150 0.997 0.425 0.443 !       0.83 eA-3
Q151 0.949 0.247 0.396 !       0.82 eA-3
C152 0.828 0.605 0.328 !       0.82 eA-3
C153 0.968 0.277 0.411 !       0.82 eA-3
Q154 0.751 0.914 0.092 !       0.81 eA-3
Q155 0.862 0.923 0.068 !       0.81 eA-3
Q156 0.826 0.017 0.323 !       0.80 eA-3
Q157 0.969 0.108 0.506 !       0.80 eA-3
C158 0.863 0.408 0.234 !       0.79 eA-3
Q159 0.267 0.836 0.042 !       0.79 eA-3
Q160 0.683 0.451 0.328 !       0.78 eA-3
C161 0.955 0.724 0.229 !       0.78 eA-3
C162 0.985 0.360 0.452 !       0.78 eA-3
Q163 0.133 0.020-0.004 !       0.77 eA-3
Q164 0.844 0.203 0.481 !       0.77 eA-3
Q165 0.969 0.222 0.425 !       0.77 eA-3
C166 0.826 0.631 0.347 !       0.76 eA-3
C167 0.151 0.546 0.383 !       0.75 eA-3
Q168 0.062 0.949 0.157 !       0.75 eA-3
C169 0.934 0.372 0.417 !       0.74 eA-3
C170 0.907 0.722 0.450 !       0.74 eA-3
Q171 0.935 1.002 0.186 !       0.74 eA-3
Q172 0.279 0.837 0.018 !       0.73 eA-3
Q173 0.237 0.796 0.485 !       0.73 eA-3
Q174 0.159 0.706 0.445 !       0.73 eA-3
C175 0.108 0.483 0.414 !       0.73 eA-3
Q176 0.831 0.097 0.446 !       0.72 eA-3
Q177 0.359 0.298 0.206 !       0.72 eA-3
Q178 0.987 0.846 0.414 !       0.72 eA-3
C179 0.781 0.622 0.378 !       0.72 eA-3
Q180 0.159 0.249 0.293 !       0.71 eA-3
C181 0.127 0.344 0.442 !       0.71 eA-3
Q182 0.784 0.028 0.341 !       0.71 eA-3
Q183 0.811 0.131 0.214 !       0.71 eA-3
Q184 0.873 0.829 0.439 !       0.71 eA-3
C185 0.066 0.581 0.440 !       0.71 eA-3
C186 0.018 0.531 0.480 !       0.71 eA-3
Q187 0.047 0.088 0.453 !       0.70 eA-3
Q188 0.174 0.672 0.067 !       0.70 eA-3
C189 0.970 0.455 0.392 !       0.70 eA-3
C190 0.852 0.453 0.274 !       0.70 eA-3
Q191 0.798 0.059 0.417 !       0.70 eA-3
Q192 0.917 0.982 0.347 !       0.69 eA-3
C193 0.892 0.512 0.278 !       0.69 eA-3
C194 0.980 0.341 0.394 !       0.69 eA-3
Q195 0.438 0.721 0.281 !       0.69 eA-3
Q196 0.732 0.144 0.078 !       0.68 eA-3
Q197 0.061 0.590 0.237 !       0.68 eA-3
Q198 0.222 0.250 0.374 !       0.68 eA-3
Q199 0.667 0.407 0.309 !       0.68 eA-3
;
_refine_diff_density_max         5.106
_refine_diff_density_min         -2.084
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1139
_refine_ls_number_reflns         26694
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0873
_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^)+(0.1672P)^2^+0.1049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2379
_refine_ls_wR_factor_ref         0.2613
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17673
_reflns_number_total             26694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00371a2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7232624--7232630.cif.'
_cod_original_cell_volume        4854.2(19)
_cod_database_code               7232625
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.993
_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, All O(H,H) groups
2. Restrained distances
 H19A-O19
 0.84 with sigma of 0.02
 H19B-O19
 0.84 with sigma of 0.02
 O18-H18B
 0.84 with sigma of 0.002
 O18-H18A
 0.84 with sigma of 0.002
 H22B-O22
 0.84 with sigma of 0.02
 H22A-O22
 0.84 with sigma of 0.002
 O17-H17B
 0.84 with sigma of 0.02
 O17-H17A
 0.84 with sigma of 0.02
 H17B-O16_$1
 1.67 with sigma of 0.02
 H22A-H22B
 1.4 with sigma of 0.04
3.a Rotating group:
 O18(H18A,H18B)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C17(H17C,H17D), C25(H25A,H25B),
 C33(H33A,H33B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C57(H57A,H57B),
  C65(H65A,H65B), C73(H73A,H73B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C11(H11), C12(H12), C14(H14), C15(H15),
 C19(H19), C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C30(H30), C31(H31),
  C35(H35), C36(H36), C38(H38), C39(H39), C42(H42), C43(H43), C45(H45),
 C46(H46), C51(H51), C52(H52), C54(H54), C55(H55), C59(H59), C60(H60), C62(H62),
  C63(H63), C67(H67), C68(H68), C70(H70), C71(H71), C75(H75), C76(H76),
 C78(H78), C79(H79), C81(H81), C84(H84), C87(H87)
3.d Idealised Me refined as rotating group:
 C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,H85B,H85C), C86(H86A,H86B,
 H86C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'