#------------------------------------------------------------------------------
#$Date: 2019-11-08 01:33:12 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/07/7700777.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_7700777
loop_
_publ_author_name
'Shi, Xing-Xing'
'Chen, Qiu-Jie'
'Chen, Xue-Li'
'Zhang, Yuexing'
'Kurmoo, Mohamedally'
'Zeng, Ming-Hua'
_publ_section_title
;
 Monitoring fragmentation and oligomerization of a di-μ-methoxo bridged
 copper(ii) complex: structure, mass spectrometry, magnetism and DFT
 studies.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13094
_journal_page_last               13100
_journal_paper_doi               10.1039/c9dt02890k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C18 H18 Cl2 Cu2 N4 O2'
_chemical_formula_sum            'C18 H18 Cl2 Cu2 N4 O2'
_chemical_formula_weight         520.34
_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   difmap
_audit_creation_date             2017-07-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2019-05-05 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                64.636(5)
_cell_angle_beta                 77.246(4)
_cell_angle_gamma                84.317(4)
_cell_formula_units_Z            1
_cell_length_a                   5.9728(2)
_cell_length_b                   8.7306(5)
_cell_length_c                   9.9516(5)
_cell_measurement_reflns_used    5031
_cell_measurement_temperature    90.15
_cell_measurement_theta_max      29.4450
_cell_measurement_theta_min      3.9640
_cell_volume                     457.34(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7873
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.977
_diffrn_reflns_theta_min         3.497
_exptl_absorpt_coefficient_mu    2.641
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.889
_exptl_crystal_description       prism
_exptl_crystal_F_000             262
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1800
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0292
_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)+(0.0280P)²+0.9216P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1712
_reflns_number_total             1800
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02890k2.cif
_cod_data_source_block           Cu2-90K
_cod_depositor_comments
'Adding full bibliography for 7700777--7700778.cif.'
_cod_database_code               7700777
_shelxl_version_number           2013-2
_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   0.879
_shelx_estimated_absorpt_t_min   0.403
_olex2_refinement_description
;
1. Restrained distances
 C4-H4
 0.95 with sigma of 0.02
 C7-H7
 0.95 with sigma of 0.02
2.a Fitted hexagon refined as free rotating group:
 C7(C8,C3,C4,C5,C6)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 1.13534(5) 0.04374(4) 0.59203(3) 0.00923(12) Uani 1 1 d .
Cl1 Cl 1.16259(11) 0.26216(8) 0.64483(7) 0.01349(16) Uani 1 1 d .
O1 O 1.0864(3) -0.1348(2) 0.5351(2) 0.0129(4) Uani 1 1 d .
N1 N 1.3674(4) -0.1169(3) 0.6867(2) 0.0106(4) Uani 1 1 d .
N2 N 1.5266(4) -0.3727(3) 0.7433(2) 0.0106(4) Uani 1 1 d .
C1 C 1.2239(4) -0.2815(3) 0.5769(3) 0.0120(5) Uani 1 1 d .
H1A H 1.321(5) -0.293(4) 0.488(3) 0.012(7) Uiso 1 1 d .
H1B H 1.132(5) -0.385(4) 0.635(4) 0.018(8) Uiso 1 1 d .
C2 C 1.3746(4) -0.2601(3) 0.6700(3) 0.0099(5) Uani 1 1 d .
H5 H 1.809(5) 0.002(4) 0.941(4) 0.023(9) Uiso 1 1 d .
H6 H 1.982(5) -0.278(4) 1.008(4) 0.019(8) Uiso 1 1 d .
C7 C 1.7941(3) -0.34738(16) 0.8973(2) 0.0149(6) Uani 1 1 d D
C8 C 1.6248(3) -0.29613(18) 0.81062(19) 0.0106(5) Uani 1 1 d G
C3 C 1.5269(2) -0.13573(19) 0.77464(18) 0.0098(5) Uani 1 1 d G
C4 C 1.5982(3) -0.02659(15) 0.8254(2) 0.0118(5) Uani 1 1 d DG
C5 C 1.7675(3) -0.07784(18) 0.9121(2) 0.0141(5) Uani 1 1 d G
C6 C 1.8655(3) -0.2382(2) 0.94807(19) 0.0157(6) Uani 1 1 d G
C9 C 1.5885(5) -0.5384(3) 0.7429(3) 0.0136(5) Uani 1 1 d .
H9A H 1.737(6) -0.535(4) 0.679(4) 0.021(8) Uiso 1 1 d .
H9B H 1.472(6) -0.569(4) 0.704(4) 0.031(9) Uiso 1 1 d .
H9C H 1.589(6) -0.620(4) 0.846(4) 0.027(9) Uiso 1 1 d .
H4 H 1.531(5) 0.078(3) 0.801(3) 0.017(8) Uiso 1 1 d D
H7 H 1.859(5) -0.452(3) 0.924(3) 0.016(8) Uiso 1 1 d 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
Cl1 Cu1 Cu1 136.81(2) . 2_756
O1 Cu1 Cu1 37.32(5) . 2_756
O1 Cu1 Cu1 37.89(5) 2_756 2_756
O1 Cu1 Cl1 98.93(6) 2_756 .
O1 Cu1 Cl1 174.11(5) . .
O1 Cu1 O1 75.21(8) 2_756 .
O1 Cu1 N1 81.67(8) . .
O1 Cu1 N1 156.39(9) 2_756 .
N1 Cu1 Cu1 118.85(7) . 2_756
N1 Cu1 Cl1 104.22(7) . .
Cu1 O1 Cu1 104.79(8) 2_756 .
C1 O1 Cu1 119.39(15) . .
C1 O1 Cu1 135.41(16) . 2_756
C2 N1 Cu1 113.39(17) . .
C2 N1 C3 105.87(19) . .
C3 N1 Cu1 140.66(15) . .
C2 N2 C8 106.45(19) . .
C2 N2 C9 127.4(2) . .
C8 N2 C9 126.0(2) . .
O1 C1 H1A 111.9(17) . .
O1 C1 H1B 112.1(18) . .
O1 C1 C2 105.4(2) . .
H1A C1 H1B 107(2) . .
C2 C1 H1A 109.1(17) . .
C2 C1 H1B 110.9(18) . .
N1 C2 N2 112.4(2) . .
N1 C2 C1 120.0(2) . .
N2 C2 C1 127.6(2) . .
C8 C7 C6 120.0 . .
C8 C7 H7 122(2) . .
C6 C7 H7 118(2) . .
N2 C8 C7 132.82(13) . .
N2 C8 C3 107.16(13) . .
C7 C8 C3 120.0 . .
N1 C3 C8 108.12(13) . .
N1 C3 C4 131.88(13) . .
C4 C3 C8 120.0 . .
C3 C4 C5 120.0 . .
C3 C4 H4 118(2) . .
C5 C4 H4 122(2) . .
C4 C5 H5 116(2) . .
C6 C5 H5 124(2) . .
C6 C5 C4 120.0 . .
C7 C6 H6 117.7(19) . .
C5 C6 H6 122.3(19) . .
C5 C6 C7 120.0 . .
N2 C9 H9A 110.9(18) . .
N2 C9 H9B 108(2) . .
N2 C9 H9C 109(2) . .
H9A C9 H9B 110(3) . .
H9A C9 H9C 111(3) . .
H9B C9 H9C 110(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu1 3.0500(6) 2_756
Cu1 Cl1 2.2129(7) .
Cu1 O1 1.9125(18) 2_756
Cu1 O1 1.9374(18) .
Cu1 N1 1.958(2) .
O1 Cu1 1.9124(18) 2_756
O1 C1 1.405(3) .
N1 C2 1.326(3) .
N1 C3 1.383(2) .
N2 C2 1.351(3) .
N2 C8 1.369(2) .
N2 C9 1.460(3) .
C1 H1A 0.98(3) .
C1 H1B 0.98(3) .
C1 C2 1.501(4) .
C7 C8 1.3900 .
C7 C6 1.3900 .
C7 H7 0.905(17) .
C8 C3 1.3900 .
C3 C4 1.3900 .
C4 C5 1.3900 .
C4 H4 0.911(17) .
C5 H5 0.93(3) .
C5 C6 1.3900 .
C6 H6 0.96(3) .
C9 H9A 0.97(3) .
C9 H9B 0.97(4) .
C9 H9C 0.97(4) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
Cu1 O1 C1 C2 174.71(17) 2_756
Cu1 O1 C1 C2 3.4(3) .
Cu1 N1 C2 N2 -176.52(16) .
Cu1 N1 C2 C1 3.7(3) .
Cu1 N1 C3 C8 175.30(19) .
Cu1 N1 C3 C4 -5.6(3) .
O1 C1 C2 N1 -4.6(3) .
O1 C1 C2 N2 175.7(2) .
N1 C3 C4 C5 -179.0(2) .
N2 C8 C3 N1 0.65(17) .
N2 C8 C3 C4 -178.55(16) .
C2 N1 C3 C8 -0.9(2) .
C2 N1 C3 C4 178.15(16) .
C2 N2 C8 C7 -178.42(16) .
C2 N2 C8 C3 -0.1(2) .
C7 C8 C3 N1 179.20(16) .
C7 C8 C3 C4 0.0 .
C8 N2 C2 N1 -0.5(3) .
C8 N2 C2 C1 179.2(2) .
C8 C7 C6 C5 0.0 .
C8 C3 C4 C5 0.0 .
C3 N1 C2 N2 0.9(3) .
C3 N1 C2 C1 -178.9(2) .
C3 C4 C5 C6 0.0 .
C4 C5 C6 C7 0.0 .
C6 C7 C8 N2 178.1(2) .
C6 C7 C8 C3 0.0 .
C9 N2 C2 N1 -176.3(2) .
C9 N2 C2 C1 3.4(4) .
C9 N2 C8 C7 -2.5(3) .
C9 N2 C8 C3 175.8(2) .
