#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:55:40 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229725 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/80/7048045.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7048045
loop_
_publ_author_name
'Kwon, Hyunchul'
'Lee, Eunsung'
_publ_section_title
;
 Fluxional motion in a dinuclear copper(i) complex with a propeller-type
 ligand: metal hopping on both sides.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17206
_journal_page_last               17210
_journal_paper_doi               10.1039/c8dt03884h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C40 H24 Cl2 Cu2 F1.03 N8'
_chemical_formula_sum            'C40 H24 Cl2 Cu2 F1.02 N8'
_chemical_formula_weight         834.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-12 deposited with the CCDC.
2018-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.75(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.939(2)
_cell_length_b                   13.812(3)
_cell_length_c                   11.949(2)
_cell_measurement_reflns_used    19538
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.508
_cell_measurement_theta_min      2.260
_cell_volume                     1796.3(6)
_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 0.985
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19538
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.260
_diffrn_source                   Synchrotron
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             842
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.769
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.357
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         5369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.357
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0478
_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/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4947
_reflns_number_total             5369
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt03884h2.cif
_cod_data_source_block           p21n70
_cod_depositor_comments          'Adding full bibliography for 7048045.cif.'
_cod_database_code               7048045
_shelx_shelxl_version_number     2016/4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.947
_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. Others
 Fixed Uiso: F1(0.04) F2(0.04) F3(0.04)
3.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17),
 C19(H19)
3.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
Cu1 Cu 0.45937(2) 0.25603(2) 0.65490(2) 0.02639(12) Uani 1 1 d .
Cl1 Cl 0.45641(5) 0.10955(4) 0.74726(5) 0.04199(17) Uani 1 1 d .
N1 N 0.56600(17) 0.23695(11) 0.52059(15) 0.0247(3) Uani 1 1 d .
N2 N 0.60176(15) 0.33407(12) 0.74029(12) 0.0260(3) Uani 1 1 d .
N3 N 0.57602(17) 0.67179(13) 0.73587(14) 0.0321(4) Uani 1 1 d .
N4 N 0.30842(16) 0.32562(13) 0.61186(14) 0.0293(3) Uani 1 1 d .
C1 C 0.51042(17) 0.59014(13) 0.71928(14) 0.0235(3) Uani 1 1 d .
C2 C 0.50677(17) 0.54461(12) 0.60536(13) 0.0225(3) Uani 1 1 d .
C3 C 0.56492(17) 0.45520(12) 0.59279(13) 0.0228(3) Uani 1 1 d .
C4 C 0.55808(16) 0.40978(12) 0.48769(13) 0.0216(3) Uani 1 1 d .
C5 C 0.64259(17) 0.41478(13) 0.69231(14) 0.0236(3) Uani 1 1 d .
C6 C 0.2243(2) 0.37215(15) 0.58456(17) 0.0330(4) Uani 1 1 d .
C7 C 0.61446(16) 0.31309(13) 0.47041(13) 0.0223(3) Uani 1 1 d .
C8 C 0.8206(2) 0.42345(16) 0.82622(17) 0.0329(4) Uani 1 1 d .
H8 H 0.895810 0.453070 0.854413 0.039 Uiso 1 1 calc R
C9 C 0.70788(16) 0.30178(16) 0.40045(14) 0.0266(4) Uani 1 1 d .
H9 H 0.743281 0.356691 0.368297 0.032 Uiso 1 1 calc R
C10 C 0.6698(2) 0.29929(16) 0.83132(16) 0.0318(4) Uani 1 1 d .
H10 H 0.641982 0.242688 0.866181 0.038 Uiso 1 1 calc R
C11 C 0.7783(2) 0.34164(17) 0.87704(16) 0.0356(4) Uani 1 1 d .
C12 C 0.6066(2) 0.14827(15) 0.49853(18) 0.0316(4) Uani 1 1 d .
H12 H 0.573193 0.094489 0.534557 0.038 Uiso 1 1 calc R
C13 C 0.4451(2) 0.54892(15) 0.80026(16) 0.0317(4) Uani 1 1 d .
H13 H 0.401587 0.489971 0.785932 0.038 Uiso 1 1 calc R
C14 C 0.75020(18) 0.46139(14) 0.73271(16) 0.0281(4) Uani 1 1 d .
H14 H 0.775688 0.518439 0.697178 0.034 Uiso 1 1 calc R
C15 C 0.5771(2) 0.71503(19) 0.8370(2) 0.0394(5) Uani 1 1 d .
H15 H 0.625044 0.771885 0.851105 0.047 Uiso 1 1 calc R
C16 C 0.5111(2) 0.67988(18) 0.92098(17) 0.0361(4) Uani 1 1 d .
C17 C 0.7483(2) 0.20991(18) 0.37848(16) 0.0329(4) Uani 1 1 d .
H17 H 0.812213 0.200770 0.331242 0.039 Uiso 1 1 calc R
C18 C 0.6949(2) 0.13114(17) 0.42587(19) 0.0358(4) Uani 1 1 d .
C19 C 0.4446(2) 0.59535(18) 0.90234(17) 0.0370(5) Uani 1 1 d .
H19 H 0.399106 0.569581 0.959127 0.044 Uiso 1 1 calc R
C20 C 0.1196(3) 0.4333(2) 0.5509(2) 0.0523(7) Uani 1 1 d .
H20A H 0.082205 0.413196 0.476588 0.078 Uiso 1 1 calc GR
H20B H 0.146652 0.500814 0.547568 0.078 Uiso 1 1 calc GR
H20C H 0.059169 0.427374 0.605733 0.078 Uiso 1 1 calc GR
F1 F 0.7403(6) 0.0521(5) 0.4169(6) 0.040 Uiso 0.210(4) 1 d .
F2 F 0.5067(8) 0.7358(5) 1.0044(7) 0.040 Uiso 0.192(4) 1 d .
F3 F 0.8248(11) 0.3132(10) 0.9606(10) 0.040 Uiso 0.110(4) 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Cu1 Cl1 106.99(5) . .
N2 Cu1 Cl1 105.43(5) . .
N2 Cu1 N1 89.65(7) . .
N4 Cu1 Cl1 120.69(6) . .
N4 Cu1 N1 112.64(7) . .
N4 Cu1 N2 116.80(7) . .
C7 N1 Cu1 121.21(13) . .
C12 N1 Cu1 119.20(14) . .
C12 N1 C7 118.30(18) . .
C5 N2 Cu1 118.94(12) . .
C10 N2 Cu1 122.65(14) . .
C10 N2 C5 117.33(17) . .
C1 N3 C15 117.52(18) . .
C6 N4 Cu1 175.15(19) . .
N3 C1 C2 116.94(15) . .
N3 C1 C13 123.34(17) . .
C13 C1 C2 119.69(16) . .
C3 C2 C1 119.73(14) . .
C3 C2 C4 120.49(15) . 3_666
C4 C2 C1 119.75(15) 3_666 .
C2 C3 C5 118.02(15) . .
C4 C3 C2 120.43(15) . .
C4 C3 C5 121.35(15) . .
C2 C4 C7 118.27(15) 3_666 .
C3 C4 C2 119.08(15) . 3_666
C3 C4 C7 122.63(14) . .
N2 C5 C3 117.34(16) . .
N2 C5 C14 122.79(16) . .
C14 C5 C3 119.86(16) . .
N4 C6 C20 178.5(3) . .
N1 C7 C4 116.78(15) . .
N1 C7 C9 121.71(18) . .
C9 C7 C4 121.41(16) . .
C11 C8 H8 120.8 . .
C11 C8 C14 118.47(19) . .
C14 C8 H8 120.8 . .
C7 C9 H9 120.4 . .
C17 C9 C7 119.11(18) . .
C17 C9 H9 120.4 . .
N2 C10 H10 118.3 . .
N2 C10 C11 123.46(19) . .
C11 C10 H10 118.3 . .
C8 C11 C10 118.84(18) . .
F3 C11 C8 121.6(7) . .
F3 C11 C10 119.2(7) . .
N1 C12 H12 118.4 . .
N1 C12 C18 123.2(2) . .
C18 C12 H12 118.4 . .
C1 C13 H13 120.8 . .
C19 C13 C1 118.43(19) . .
C19 C13 H13 120.8 . .
C5 C14 C8 119.10(18) . .
C5 C14 H14 120.5 . .
C8 C14 H14 120.5 . .
N3 C15 H15 118.7 . .
N3 C15 C16 122.5(2) . .
C16 C15 H15 118.7 . .
C15 C16 C19 119.00(19) . .
F2 C16 C15 115.0(4) . .
F2 C16 C19 125.5(4) . .
C9 C17 H17 120.3 . .
C9 C17 C18 119.33(19) . .
C18 C17 H17 120.3 . .
C12 C18 C17 118.2(2) . .
F1 C18 C12 122.0(4) . .
F1 C18 C17 118.7(4) . .
C13 C19 C16 119.14(19) . .
C13 C19 H19 120.4 . .
C16 C19 H19 120.4 . .
C6 C20 H20A 109.5 . .
C6 C20 H20B 109.5 . .
C6 C20 H20C 109.5 . .
H20A C20 H20B 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cl1 2.3063(6) .
Cu1 N1 2.0929(19) .
Cu1 N2 2.0762(18) .
Cu1 N4 1.9352(17) .
N1 C7 1.345(2) .
N1 C12 1.338(2) .
N2 C5 1.350(2) .
N2 C10 1.344(2) .
N3 C1 1.341(2) .
N3 C15 1.347(3) .
N4 C6 1.143(3) .
C1 C2 1.496(2) .
C1 C13 1.382(3) .
C2 C3 1.404(2) .
C2 C4 1.407(2) 3_666
C3 C4 1.399(2) .
C3 C5 1.498(2) .
C4 C2 1.407(2) 3_666
C4 C7 1.494(2) .
C5 C14 1.385(3) .
C6 C20 1.447(3) .
C7 C9 1.392(2) .
C8 H8 0.9500 .
C8 C11 1.384(3) .
C8 C14 1.394(3) .
C9 H9 0.9500 .
C9 C17 1.378(3) .
C10 H10 0.9500 .
C10 C11 1.386(3) .
C11 F3 1.143(13) .
C12 H12 0.9500 .
C12 C18 1.382(3) .
C13 H13 0.9500 .
C13 C19 1.379(3) .
C14 H14 0.9500 .
C15 H15 0.9500 .
C15 C16 1.381(3) .
C16 C19 1.382(3) .
C16 F2 1.266(8) .
C17 H17 0.9500 .
C17 C18 1.383(3) .
C18 F1 1.208(7) .
C19 H19 0.9500 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
