Static and dynamic coordination behaviours of copper(i) ions in hexa(2-pyridyl)benzene ligand systems.
Kwon, Hyunchul; Lee, Eunsung; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8448–8455; doi:10.1039/c8dt01424h

data_7046534
_publ_section_title
;
 Static and dynamic coordination behaviours of copper(i) ions in
 hexa(2-pyridyl)benzene ligand systems.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8448
_journal_page_last               8455
_journal_paper_doi               10.1039/c8dt01424h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C44 H39 Cl Cu N7, 2(C2 H3 N)'
_chemical_formula_sum            'C48 H45 Cl Cu N9'
_chemical_formula_weight         846.92
_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   geom
_audit_creation_date             2018-05-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2018-05-05 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.20(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.704(5)
_cell_length_b                   14.101(3)
_cell_length_c                   27.437(6)
_cell_measurement_reflns_used    23620
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.575
_cell_measurement_theta_min      1.563
_cell_volume                     8712(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            23620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         1.563
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.607
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dull yellow'
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.726
_refine_diff_density_min         -1.877
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         12165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0859
_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^)+(0.0772P)^2^+69.4714P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2237
_refine_ls_wR_factor_ref         0.2273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10829
_reflns_number_total             12165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01424h2.cif
_cod_data_source_block           output
_cod_depositor_comments
'Adding full bibliography for 7046531--7046536.cif.'
_cod_original_cell_volume        8712(3)
_cod_database_code               7046534
_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 C(H,H,H) groups
2. Shared sites
{N7, C1A}
{C35, N35}
3. Uiso/Uaniso restraints and constraints
Uanis(N7) = Uanis(C1A)
Uanis(C35) = Uanis(N35)
4. Others
 Fixed Sof: N7(0.5) C35(0.5) H35(0.5) C1A(0.5) H1A(0.5) N35(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C9(H9), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19),
 C20(H20), C22(H22), C25(H25), C26(H26), C32(H32), C35(H35), C37(H37), C38(H38),
  C41(H41), C44(H44), C1A(H1A)
5.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C)
;
_olex2_submission_special_instructions 'No special instructions were received'