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_7702532
_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 H30 Cl2 N6 O9 Zn'
_chemical_formula_sum            'C18 H30 Cl2 N6 O9 Zn'
_chemical_formula_weight         610.75
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 98.749(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5701(5)
_cell_length_b                   15.8048(9)
_cell_length_c                   15.2231(6)
_cell_measurement_reflns_used    10613
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     2513.6(2)
_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
;
10613 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   40 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta ==    6.30 Omega ==    0.00 Kappa ==    0.00  112 frames
Set 2 Theta ==   -6.30 Kappa ==  129.00 Phi   ==    0.00   18 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       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10613
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.61
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.010
_refine_diff_density_min         -0.385
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   7.097
_refine_ls_goodness_of_fit_ref   1.224
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3488
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.084
_refine_ls_R_factor_gt           0.045
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.363
_refine_ls_wR_factor_ref         0.066
_reflns_number_gt                3488
_reflns_number_total             5974
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b010074i.txt
_cod_data_source_block           complex_5_[Cupytrien](ClO4)2_H2O_(5)
_cod_original_cell_volume        2513.6(4)
_cod_database_code               7702532