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_7702781
_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 H24 N6 Ni O3'
_chemical_formula_sum            'C18 H24 N6 Ni O3'
_chemical_formula_weight         431.14
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             19-02-02
_cell_angle_alpha                90
_cell_angle_beta                 101.582(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1934(3)
_cell_length_b                   12.1481(3)
_cell_length_c                   15.4149(5)
_cell_measurement_reflns_used    6969
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     1869.97(10)
_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
;
6969 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   87 frames
Friedel pairs were averaged. Internal R = 0.03
;
_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  0.030
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6969
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.53
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.453
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.548
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3114
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.057
_refine_ls_wR_factor_ref         0.037
_reflns_number_gt                3114
_reflns_number_total             4363
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b111614b.txt
_cod_data_source_block           complex_5:
_cod_original_cell_volume        1869.97(9)
_cod_database_code               7702781