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_7231247
_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, 5.5(H2 O)'
_chemical_formula_sum            'C36 H39 Cl4 Cu2 N6 O7.5'
_chemical_formula_weight         944.61
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-10
_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                113.957(18)
_cell_angle_beta                 111.576(17)
_cell_angle_gamma                91.514(16)
_cell_formula_units_Z            1
_cell_length_a                   9.081(5)
_cell_length_b                   10.926(6)
_cell_length_c                   12.055(7)
_cell_measurement_reflns_used    4501
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.228
_cell_measurement_theta_min      2.031
_cell_volume                     994.5(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27505
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.228
_diffrn_reflns_theta_max         25.228
_diffrn_reflns_theta_min         2.031
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1537 before and 0.0926 after correction.
The Ratio of minimum to maximum transmission is 0.6473.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       block
_exptl_crystal_F_000             483
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3561
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0557P)^2^+3.7812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2859
_reflns_number_total             3561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00918j2.cif
_cod_data_source_block           p-1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7231245--7231248.cif.'
_cod_original_cell_volume        994.5(9)
_cod_original_formula_sum        'C36 H39 Cl4 Cu2 N6 O7.50'
_cod_database_code               7231247
_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. Restrained distances
 O1-H1A = O1-H1B
 0.84 with sigma of 0.01
 O4-H4A
 0.95 with sigma of 0.01
 O4-H4B
 0.95 with sigma of 0.01
 O2-H2A
 1 with sigma of 0.02
 H1A-H1B
 1.34 with sigma of 0.02
3. Others
 Fixed Sof: O4(0.75) H4A(0.75) H4B(0.75)
4.a Free rotating group:
 O2(H2A,H2B), O4(H4A,H4B), O3(H3A,H3B)
4.b Rotating group:
 O1(H1A,H1B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C3(H3), C9(H9), C12(H12), C2(H2), C15(H15), C10(H10),
 C11(H11), C16(H16), C18(H18), C17(H17)
;
_olex2_submission_special_instructions 'No special instructions were received'