Structural effects of potentially hexadentate N4O2, N4S2 or N6 ligands involving pyridine, amine and ether or thioether donors: crystal structure of copper(II) and zinc(II) complexes †
Jubert, Caroline; Mohamadou, Aminou; Marrot, Jérôme; Barbier, Jean-Pierre; Journal of the Chemical Society, Dalton Transactions  (2001) 1230–; doi:10.1039/b010074i

data_7702531
_publ_section_title
;
 Structural effects of potentially hexadentate N4O2, N4S2 or N6 ligands
 involving pyridine, amine and ether or thioether donors: crystal
 structure of copper(II) and zinc(II) complexes&#x200A;&#x2020;
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1230
_journal_paper_doi               10.1039/b010074i
_journal_year                    2001
_chemical_formula_moiety         'C18 H28 Cl2 N4 O11 Zn'
_chemical_formula_sum            'C18 H28 Cl2 N4 O11 Zn'
_chemical_formula_weight         612.72
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                94.039(5)
_cell_angle_beta                 99.520(5)
_cell_angle_gamma                107.008(5)
_cell_formula_units_Z            2
_cell_length_a                   9.3266(5)
_cell_length_b                   11.6770(5)
_cell_length_c                   12.2295(5)
_cell_measurement_temperature    173
_cell_volume                     1246.08(11)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
8342 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance ==  36. mm.
Scan angle ==  2.0 deg 1 scans of   30 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta ==    6.40 Omega ==    0.00 Kappa ==    0.00   91 frames
Set 2 Theta ==   -6.40 Kappa == -174.00 Phi   ==    0.00   22 frames
Friedel pairs were averaged. Internal R == 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8342
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.264
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.63
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.249
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   14.957
_refine_ls_goodness_of_fit_ref   1.332
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3514
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.093
_refine_ls_R_factor_gt           0.055
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.824
_refine_ls_wR_factor_ref         0.080
_reflns_number_gt                3514
_reflns_number_total             5674
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b010074i.txt
_cod_data_source_block           complex_3_[Znpydado](ClO4)2_H2O_(3)
_cod_original_cell_volume        1246.1(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702531