Monitoring fragmentation and oligomerization of a di-μ-methoxo bridged copper(ii) complex: structure, mass spectrometry, magnetism and DFT studies.
Shi, Xing-Xing; Chen, Qiu-Jie; Chen, Xue-Li; Zhang, Yuexing; Kurmoo, Mohamedally; Zeng, Ming-Hua; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13094–13100; doi:10.1039/c9dt02890k

data_7700777
_publ_section_title
;
 Monitoring fragmentation and oligomerization of a di-\m-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       '\w 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/[\s^2^(Fo^2^)+(0.0280P)^2^+0.9216P]
 where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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)
;
_shelx_res_checksum              28047
_olex2_submission_special_instructions 'No special instructions were received'