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_7232630
_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         'C43 H40 Cu2 N3 O9.5'
_chemical_formula_sum            'C43 H40 Cu2 N3 O9.5'
_chemical_formula_weight         877.86
_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
_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                101.03(3)
_cell_angle_beta                 106.14(3)
_cell_angle_gamma                94.29(3)
_cell_formula_units_Z            2
_cell_length_a                   10.954(2)
_cell_length_b                   13.627(3)
_cell_length_c                   14.312(3)
_cell_measurement_reflns_used    13813
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.078
_cell_measurement_theta_min      1.907
_cell_volume                     1995.6(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.843
_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  0.2504
_diffrn_reflns_av_unetI/netI     0.0895
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            133265
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         34.078
_diffrn_reflns_theta_min         1.907
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.127
_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    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             906
_exptl_crystal_recrystallization_method 'From reaction mixture'
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.382
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         13813
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0657
_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^)+(0.1049P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8720
_reflns_number_total             13813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00371a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7232624--7232630.cif.'
_cod_original_formula_sum        'C43 H40 Cu2 N3 O9.50'
_cod_database_code               7232630
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.978
_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
 C40-C39A \\sim C40-C39B
 with sigma of 0.04
 C39A-C33A \\sim C39B-C33A
 with sigma of 0.04
 C26A-C31A \\sim C26B-C31B
 with sigma of 0.02
 C26A-C27A \\sim C26B-C27B
 with sigma of 0.02
 C26A-C25A \\sim C26B-C25A
 with sigma of 0.02
 C32-C31A \\sim C32-C31B
 with sigma of 0.04
 C32-C29A \\sim C32-C29B
 with sigma of 0.04
 C31A-C29A \\sim C31B-C29B
 with sigma of 0.04
 C31A-C27A \\sim C31B-C27B
 with sigma of 0.04
 C31A-C25A \\sim C31B-C25A
 with sigma of 0.04
 C29A-C27A \\sim C29B-C27B
 with sigma of 0.04
 C27A-C25A \\sim C27B-C25A
 with sigma of 0.04
 C29A-C28A \\sim C29B-C28B
 with sigma of 0.02
 C28A-C27A \\sim C28B-C27B
 with sigma of 0.02
 C26A-C28A \\sim C26B-C28B
 with sigma of 0.04
 C7A-C6A \\sim C7B-C6B
 with sigma of 0.02
 C6A-C5A \\sim C6B-C5B
 with sigma of 0.02
 C4A-C5A \\sim C4B-C5B
 with sigma of 0.02
 N2-C5A \\sim N2-C5B
 with sigma of 0.04
 C7A-C5A \\sim C7B-C5B
 with sigma of 0.04
 C6A-C4A \\sim C6B-C4B
 with sigma of 0.04
 C36A-C35A \\sim C36B-C35B
 with sigma of 0.02
 C39A-C35A \\sim C39B-C35B
 with sigma of 0.04
 C35A-C33A \\sim C35B-C33A
 with sigma of 0.04
 C37A-C36A \\sim C37B-C36B
 with sigma of 0.02
 C37A-C40 \\sim C37B-C40
 with sigma of 0.04
 C37A-C39A \\sim C37B-C39B
 with sigma of 0.04
 C37A-C35A \\sim C37B-C35B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C34B \\sim C35B \\sim C36B \\sim C37B \\sim C38 \\sim C39B: within 1.7A with
sigma of 0.004 and sigma for terminal atoms of 0.08
Uanis(C28B) \\sim Ueq, Uanis(C29B) \\sim Ueq, Uanis(C31B) \\sim Ueq,
Uanis(C26B) \\sim Ueq, Uanis(C27B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C7B) \\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C4B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O10(0.5) H10A(0.5) H10B(0.5) C0AA(0.25) H0AA(0.25) H0AB(0.25)
 H3A(0.75) H3B(0.25) C4A(0.75) H4A(0.75) C4B(0.25) H4B(0.25) C5A(0.75)
 C5B(0.25) C6A(0.75) H6A(0.75) C6AA(0.25) H6AA(0.25) H6AB(0.25) C6B(0.25)
 H6B(0.25) C7A(0.75) H7A(0.75) C7B(0.25) H7B(0.25) C8A(0.75) H8AA(0.75)
 H8AB(0.75) C8B(0.25) H8BA(0.25) H8BB(0.25) C25A(0.75) H25A(0.75) H25B(0.75)
 C26A(0.75) C31A(0.75) H31A(0.75) C29A(0.75) H29A(0.75) C28A(0.75) H28A(0.75)
 C27A(0.75) H27A(0.75) C26B(0.25) C27B(0.25) H27B(0.25) C28B(0.25) H28B(0.25)
 C29B(0.25) H29B(0.25) C31B(0.25) H31B(0.25) C33A(0.75) H33A(0.75) H33B(0.75)
 C34A(0.75) C34B(0.25) C35A(0.75) H35A(0.75) C35B(0.25) H35B(0.25) C36A(0.75)
 H36A(0.75) C36B(0.25) H36B(0.25) C37A(0.75) H37A(0.75) C37B(0.25) H37B(0.25)
 C39A(0.75) H39A(0.75) C39B(0.25) H39B(0.25)
5.a Rotating group:
 O10(H10A,H10B)
5.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1(H1A,H1B), C6AA(H6AA,H6AB), C8A(H8AA,H8AB), C8B(H8BA,H8BB),
  C9(H9A,H9B), C17(H17A,H17B), C25A(H25A,H25B), C33A(H33A,H33B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C3(H3B), C4A(H4A), C4B(H4B), C6A(H6A), C6B(H6B), C7A(H7A), C7B(H7B),
 C11(H11), C12(H12), C13(H13), C15(H15), C19(H19), C20(H20), C21(H21), C23(H23),
  C31A(H31A), C29A(H29A), C28A(H28A), C27A(H27A), C27B(H27B), C28B(H28B),
 C29B(H29B), C31B(H31B), C35A(H35A), C35B(H35B), C36A(H36A), C36B(H36B),
 C37A(H37A), C37B(H37B), C39A(H39A), C39B(H39B), C41(H41)
5.d Fitted hexagon refined as free rotating group:
 C26A(C31A,C30,C29A,C28A,C27A)
5.e Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C)
;
_olex2_submission_special_instructions 'No special instructions were received'