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_7702782
_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         'C36 H54 Cl2 Co2 N12 O15'
_chemical_formula_sum            'C36 H54 Cl2 Co2 N12 O15'
_chemical_formula_weight         1083.68
_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'
_audit_creation_date             19-02-02
_cell_angle_alpha                75.898(5)
_cell_angle_beta                 71.629(5)
_cell_angle_gamma                71.844(5)
_cell_formula_units_Z            2
_cell_length_a                   11.6623(3)
_cell_length_b                   13.0775(3)
_cell_length_c                   16.7715(5)
_cell_measurement_reflns_used    10272
_cell_measurement_temperature    294
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     2276.46(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      294
_diffrn_measurement_details
;
10272 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  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    5.90 Omega =    0.00 Kappa =    0.00   91 frames
Set 2 Theta =   -3.90 Kappa = -172.00 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       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10272
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.58
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   8.421
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     576
_refine_ls_number_reflns         5852
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.129
_refine_ls_R_factor_gt           0.067
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.024
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.492
_refine_ls_wR_factor_ref         0.077
_reflns_number_gt                5852
_reflns_number_total             10272
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b111614b.txt
_cod_data_source_block           complex_6:
_cod_original_cell_volume        2276.5(1)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702782