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_7232627
_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 H41 Cu2 N3 O10, C3 H7 N O'
_chemical_formula_sum            'C46 H48 Cu2 N4 O11'
_chemical_formula_weight         959.96
_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                 107.55(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.007(5)
_cell_length_b                   34.875(7)
_cell_length_c                   16.063(3)
_cell_measurement_reflns_used    11371
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.862
_cell_measurement_theta_min      1.035
_cell_volume                     13357(5)
_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      100.0
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1053
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            41996
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        24.862
_diffrn_reflns_theta_max         24.862
_diffrn_reflns_theta_min         1.035
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.955
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_recrystallization_method 'From reaction mixture'
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_platon_squeeze_details          (replace
_refine_diff_density_max         1.078
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     580
_refine_ls_number_reflns         11371
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1204
_refine_ls_R_factor_gt           0.0812
_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^)+(0.1657P)^2^+3.7227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2369
_refine_ls_wR_factor_ref         0.2629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7119
_reflns_number_total             11371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00371a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7232624--7232630.cif.'
_cod_database_code               7232627
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.980
_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
2. Restrained distances
 H10A-O10
 0.84 with sigma of 0.002
 H10B-O10
 0.84 with sigma of 0.02
 H10B-O11
 1.935 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C9(H9A,H9B), C17(H17A,H17B), C25(H25A,H25B),
 C33(H33A,H33B)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), 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), C41(H41), C44(H44)
4.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C)
;
_olex2_submission_special_instructions 'No special instructions were received'