Coordination preference of hexa(2-pyridyl)benzene with copper(ii) directed by hydrogen bonding
Kwon, Hyunchul; Lee, Eunsung; CrystEngComm 20 (2018) 5233–; doi:10.1039/C8CE00918J

data_7231245
_publ_section_title
;
 Coordination preference of hexa(2-pyridyl)benzene with copper(ii)
 directed by hydrogen bonding
;
_journal_issue                   35
_journal_name_full               CrystEngComm
_journal_page_first              5233
_journal_paper_doi               10.1039/C8CE00918J
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C36 H28 Cl4 Cu2 N6 O2, 4.75(H2 O)'
_chemical_formula_sum            'C36 H37.5 Cl4 Cu2 N6 O6.75'
_chemical_formula_weight         931.10
_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             2018-07-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-07-17 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                94.72(3)
_cell_angle_beta                 115.28(3)
_cell_angle_gamma                114.86(3)
_cell_formula_units_Z            2
_cell_length_a                   12.509(3)
_cell_length_b                   13.689(3)
_cell_length_c                   14.613(3)
_cell_measurement_reflns_used    12849
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.021
_cell_measurement_theta_min      1.626
_cell_volume                     1945.6(13)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.63000
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.940
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_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            12849
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         1.626
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             951
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.280
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         7197
_refine_ls_number_restraints     402
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4817
_reflns_number_total             7197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00918j2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7231245--7231248.cif.'
_cod_original_cell_volume        1945.6(9)
_cod_original_formula_sum        'C36 H37.50 Cl4 Cu2 N6 O6.75'
_cod_database_code               7231245
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33,
  C34, C35, C36, N1, N2, N3, N4, N5, N6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5
\\sim N6: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Fixed Sof: O3(0.75) H3A(0.75) H3B(0.75) O4(0.75) H4A(0.75) H4B(0.75) O5(0.75)
 H5A(0.75) H5B(0.75) O6(0.75) H6B(0.75) H6A(0.75) O8(0.75) H8A(0.75) H8B(0.75)
5.a Free rotating group:
 O7(H7B,H7A), O3(H3A,H3B), O4(H4A,H4B), O5(H5A,H5B), O6(H6B,H6A), O8(H8A,H8B)
5.b Rotating group:
 O1(H1A,H1B), O2(H2A,H2B)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'