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_7232626
_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         'C20 H18 Cu N O5'
_chemical_formula_sum            'C20 H18 Cu N O5'
_chemical_formula_weight         415.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 93.12(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.204(4)
_cell_length_b                   13.645(5)
_cell_length_c                   22.195(4)
_cell_measurement_reflns_used    3347
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.255
_cell_measurement_theta_min      1.952
_cell_volume                     4900(2)
_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 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'ADSC Quantum 315r'
_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  0.3138
_diffrn_reflns_av_unetI/netI     0.1729
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19498
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        23.258
_diffrn_reflns_theta_max         23.258
_diffrn_reflns_theta_min         1.953
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_recrystallization_method 'From reaction mixture'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_platon_squeeze_details
;
TITL 2 P -1 R = New: C2/c
CELL   16.2040   13.6450   22.1950     90.00     93.12     90.00
SPGR C2/c
Q101 0.758 0.271 0.489 !       3.39 eA-3
C102 0.500 0.297 0.250 !       2.98 eA-3
Q103 0.577 0.076 0.083 !       2.58 eA-3
Q104 0.861 0.345 0.487 !       2.03 eA-3
C105 0.561 0.321 0.258 !       1.90 eA-3
C106 0.083 0.858 0.248 !       1.71 eA-3
C107 0.583 0.358 0.248 !       1.71 eA-3
C108 0.425 0.159 0.406 !       1.70 eA-3
C109 0.450 0.111 0.423 !       1.55 eA-3
C110 0.514 0.035 0.406 !       1.55 eA-3
C111 0.396 0.340 0.267 !       1.47 eA-3
C112 0.478 0.078 0.411 !       1.46 eA-3
Q113 0.228 0.375 0.015 !       1.37 eA-3
C114 0.993 0.453 0.321 !       1.34 eA-3
C115 0.497 0.127 0.242 !       1.32 eA-3
C116 0.429 0.204 0.288 !       1.24 eA-3
Q117 0.878 0.495 0.443 !       1.24 eA-3
C118 0.034 0.486 0.158 !       1.23 eA-3
C119 0.533 0.187 0.261 !       1.18 eA-3
C120 0.436 0.262 0.317 !       1.18 eA-3
C121 0.385 0.294 0.304 !       1.17 eA-3
C122 0.564 0.139 0.175 !       1.13 eA-3
C123 0.500 0.188 0.255 !       1.11 eA-3
C124 0.581 0.267 0.212 !       1.11 eA-3
C125 0.621 0.235 0.163 !       1.06 eA-3
C126 0.494 0.014 0.161 !       1.04 eA-3
Q127 0.377 0.174 0.336 !       1.01 eA-3
Q128 0.429 0.329 0.040 !       0.99 eA-3
C129 0.406 0.215 0.329 !       0.99 eA-3
C130 0.936 0.374 0.309 !       0.98 eA-3
C131 0.513 0.243 0.307 !       0.97 eA-3
C132 0.372 0.236 0.313 !       0.97 eA-3
C133 0.624 0.282 0.175 !       0.97 eA-3
C134 0.504 0.201 0.282 !       0.95 eA-3
Q135 0.084 0.437 0.086 !       0.95 eA-3
C136 0.987 0.385 0.319 !       0.95 eA-3
C137 0.629 0.372 0.264 !       0.94 eA-3
C138 0.535 0.239 0.171 !       0.94 eA-3
Q139 0.672 0.058 0.429 !       0.90 eA-3
Q140 0.705 0.157 0.388 !       0.90 eA-3
C141 0.546 0.047 0.163 !       0.90 eA-3
C142 0.040 0.424 0.162 !       0.89 eA-3
Q143 0.083 0.174 0.365 !       0.88 eA-3
Q144 0.549 0.308 0.490 !       0.88 eA-3
Q145 0.145 0.279 0.012 !       0.87 eA-3
C146 0.973 0.485 0.223 !       0.86 eA-3
C147 0.446 0.293 0.296 !       0.86 eA-3
C148 0.474 0.154 0.282 !       0.84 eA-3
C149 0.548 0.144 0.135 !       0.82 eA-3
C150 0.554 0.250 0.282 !       0.81 eA-3
C151 0.500 0.031 0.249 !       0.80 eA-3
Q152 0.140 0.205 0.320 !       0.79 eA-3
C153 0.527 0.078 0.142 !       0.79 eA-3
Q154 0.424 0.472 0.371 !       0.79 eA-3
Q155 0.388 0.438 0.101 !       0.79 eA-3
C156 0.479 0.157 0.218 !       0.79 eA-3
C157 0.012 0.436 0.232 !       0.77 eA-3
C158 0.942 0.471 0.315 !       0.77 eA-3
C159 0.556 0.201 0.136 !       0.76 eA-3
C160 0.989 0.437 0.263 !       0.76 eA-3
C161 0.114 0.452 0.391 !       0.75 eA-3
C162 0.337 0.265 0.360 !       0.75 eA-3
Q163 0.539 0.395 0.452 !       0.75 eA-3
C164 0.076 0.358 0.157 !       0.75 eA-3
Q165 0.356 0.391 0.031 !       0.74 eA-3
Q166 0.342 0.067 0.106 !       0.73 eA-3
Q167 0.292 0.143 0.140 !       0.72 eA-3
Q168 0.644 0.098 0.421 !       0.72 eA-3
Q169 0.579 0.093 0.035 !       0.71 eA-3
C170 0.950 0.496 0.201 !       0.71 eA-3
C171 0.672 0.267 0.117 !       0.71 eA-3
Q172 0.410 0.062 0.091 !       0.70 eA-3
C173 0.657 0.357 0.237 !       0.70 eA-3
Q174 0.710 0.080 0.291 !       0.69 eA-3
Q175 0.171 0.139 0.264 !       0.69 eA-3
Q176 0.734 0.067 0.428 !       0.69 eA-3
C177 0.508 0.310 0.302 !       0.68 eA-3
C178 0.032 0.406 0.255 !       0.68 eA-3
Q179 0.667 0.330 0.466 !       0.68 eA-3
Q180 0.599 0.016 0.376 !       0.68 eA-3
C181 0.501 0.078 0.178 !       0.67 eA-3
C182 0.429 0.141 0.297 !       0.67 eA-3
Q183 0.277 0.199 0.109 !       0.67 eA-3
C184 0.473 0.093 0.089 !       0.67 eA-3
Q185 0.545 0.388 0.307 !       0.67 eA-3
Q186 0.702 0.053 0.199 !       0.67 eA-3
Q187 0.066 0.188 0.417 !       0.66 eA-3
Q188 0.407 0.488 0.411 !       0.66 eA-3
Q189 0.288 0.095 0.159 !       0.66 eA-3
C190 0.960 0.482 0.276 !       0.66 eA-3
Q191 0.364 0.467 0.432 !       0.66 eA-3
Q192 0.298 0.030 0.219 !       0.65 eA-3
Q193 0.803 0.481 0.282 !       0.65 eA-3
Q194 0.336 0.268 0.290 !       0.65 eA-3
Q195 0.279 0.061 0.261 !       0.65 eA-3
Q196 0.680 0.218 0.152 !       0.65 eA-3
Q197 0.111 0.484 0.337 !       0.65 eA-3
Q198 0.909 0.456 0.204 !       0.64 eA-3
C199 0.499 0.469 0.255 !       0.64 eA-3
;
_refine_diff_density_max         2.789
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3347
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.1669
_refine_ls_R_factor_gt           0.1361
_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          0.3374
_refine_ls_wR_factor_ref         0.3617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2086
_reflns_number_total             3347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00371a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7232624--7232630.cif.'
_cod_database_code               7232626
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.982
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 H5B-O5
 0.84 with sigma of 0.002
 H5A-O5
 0.84 with sigma of 0.002
 H5B-H5A
 1.4 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5C,H5D), C13(H13A,H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C11(H11), C15(H15), C16(H16),
 C17(H17), C19(H19)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'