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_7232624
_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         '2(Cl), 2(C20 H19 N O4)'
_chemical_formula_sum            'C40 H38 Cl2 N2 O8'
_chemical_formula_weight         745.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-04
_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                 105.68(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.074(4)
_cell_length_b                   12.547(3)
_cell_length_c                   14.060(3)
_cell_measurement_reflns_used    7810
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.932
_cell_measurement_theta_min      1.004
_cell_volume                     3579.3(14)
_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 0.995
_diffrn_measured_fraction_theta_max 0.993
_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  0.0454
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33157
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.935
_diffrn_reflns_theta_min         1.004
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1560
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water, HCl'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         8524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0159P)^2^+19.2863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1923
_refine_ls_wR_factor_ref         0.1940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7805
_reflns_number_total             8524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00371a2.cif
_cod_data_source_block           h6p4pxycl2
_cod_depositor_comments
'Adding full bibliography for 7232624--7232630.cif.'
_cod_original_cell_volume        3579.3(13)
_cod_database_code               7232624
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.995
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1A), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1B,H1C), C5(H5A,H5B), C13(H13A,H13B), C21(H21A,H21B), C25(H25A,H25B),
 C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C15(H15), C16(H16),
 C18(H18), C19(H19), C23(H23), C24(H24), C27(H27), C28(H28), C30(H30), C31(H31),
  C35(H35), C36(H36), C38(H38), C39(H39)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O3(H3), O5(H5), O7(H7A)
;
_shelx_res_checksum              10348
_olex2_submission_special_instructions 'No special instructions were received'