Equilibrium and structural studies of complexes with a hexadentate ligand containing amide, amine and pyridyl nitrogen donors. Crystal structures of copper(ii), nickel(ii) and cobalt(iii) complexes
Jubert, Caroline; Mohamadou, Aminou; Gérard, Christian; Brandes, Stéphane; Tabard, Alain; Barbier, Jean-Pierre; Journal of the Chemical Society, Dalton Transactions  (2002) 2660–; doi:10.1039/b111614b

data_7702780
_publ_section_title
;
 Equilibrium and structural studies of complexes with a hexadentate ligand
 containing amide, amine and pyridyl nitrogen donors. Crystal structures
 of copper(ii), nickel(ii) and cobalt(iii) complexes
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2660
_journal_paper_doi               10.1039/b111614b
_journal_year                    2002
_chemical_formula_moiety         'C18 H27 Cl Cu N6 O8'
_chemical_formula_sum            'C18 H27 Cl Cu N6 O8'
_chemical_formula_weight         554.44
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.4288(1)
_cell_length_b                   20.6531(4)
_cell_length_c                   30.1017(6)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     4618.44(14)
_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
;
9946 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   60 sec per frame.
Data collection was divided into  1 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00  166 frames
Friedel pairs were averaged. Internal R = 0.06
;
_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  0.060
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            9946
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.119
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.59
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   40.905
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     307
_refine_ls_number_reflns         2832
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.103
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.016
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         1.699
_refine_ls_wR_factor_ref         0.059
_reflns_number_gt                2832
_reflns_number_total             5844
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b111614b.txt
_cod_data_source_block           Complex4:
_cod_original_cell_volume        4618.4(1)
_cod_database_code               7702780