Synthesis, structure, thermal, magnetic properties and quantum mechanical calculations of bridged [bis(di(2-methylpyridyl)amine)-(μ2-1,2-bis(4-pyridyl)ethane)-tetraperchlorato-dicopper(ii)] dihydrate complex
Massoud, Salah S.; Taylor, Eric; Liu, Yuemin; Grebowicz, Janusz; Vicente, Ramon; Lalancette, Roger; Mukhopadhyay, Udai; Bernal, Ivan; Watkins, Steven F.; CrystEngComm 16 (2014) 175–; doi:10.1039/c3ce41821a

data_7213563
_publ_section_title
;
 Synthesis, structure, thermal, magnetic properties and quantum mechanical
 calculations of bridged
 [bis(di(2-methylpyridyl)amine)-(\m2-1,2-bis(4-pyridyl)ethane)-tetraperchlorato-dicopper(ii)]
 dihydrate complex
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              175
_journal_paper_doi               10.1039/c3ce41821a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         '(C36 H38 N8 Cu2 4+) 4(Cl O4 1-) 2(H2 O)'
_chemical_formula_sum            'C36 H42 Cl4 Cu2 N8 O18'
_chemical_formula_weight         1143.67
_chemical_name_systematic
;
Bis[di(2-pyridylmethyl)aminecopper(II)]-(\m~2~-1,2-bis(4-pyridyl)ethane)
Tetraperchlorate Dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-16T14:39:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.265(14)
_cell_angle_beta                 82.354(14)
_cell_angle_gamma                79.121(11)
_cell_formula_units_Z            3
_cell_length_a                   22.228(8)
_cell_length_b                   8.878(3)
_cell_length_c                   17.393(5)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      2.09
_cell_volume                     3337.9(19)
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, 2008), 
IDEAL (Gould et al., 1988)
;
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Saturn 724 with CCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26898
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.281
_exptl_absorpt_correction_T_max  0.9045
_exptl_absorpt_correction_T_min  0.6627
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lathe
_exptl_crystal_F_000             1770
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.57
_refine_diff_density_min         -1.911
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     920
_refine_ls_number_reflns         12051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_gt           0.0771
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1111P)^2^+6.5239P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2206
_reflns_number_gt                9988
_reflns_number_total             12051
_reflns_threshold_expression     I>2s\(I)
_cod_data_source_file            c3ce41821a.txt
_cod_data_source_block           cu100
_cod_original_cell_volume        3338.0(19)
_cod_database_code               7213563