Seven-coordination versus six-coordination in divalent first-row transition-metal complexes derived from 1,10-diaza-15-crown-5.
Vaiana, Lea; Regueiro-Figueroa, Martín; Mato-Iglesias, Marta; Platas-Iglesias, Carlos; Esteban-Gómez, David; de Blas, Andrés; Rodríguez-Blas, Teresa; Inorganic chemistry 46 (2007) 8271–8282; doi:10.1021/ic7008946

data_4339477
_publ_section_title
;
 Seven-coordination versus six-coordination in divalent first-row
 transition-metal complexes derived from 1,10-diaza-15-crown-5.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8271
_journal_page_last               8282
_journal_paper_doi               10.1021/ic7008946
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H34 N6 Ni O3, 2(Cl O4), H2 O '
_chemical_formula_sum            'C26 H36 Cl2 N6 Ni O12'
_chemical_formula_weight         754.22
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2007-02-26T21:20:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.266(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4318(3)
_cell_length_b                   17.0988(4)
_cell_length_c                   15.6524(4)
_cell_measurement_reflns_used    6517
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      21.585
_cell_measurement_theta_min      2.25
_cell_measurement_wavelength     0.71073
_cell_volume                     3057.18(13)
_computing_cell_refinement       'BRUKER APEX'
_computing_data_collection       'BRUKER APEX'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    DIRDIF99
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1047
_diffrn_reflns_av_unetI/netI     0.1014
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30237
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.85
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6285
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1784
_reflns_number_gt                3825
_reflns_number_total             6285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7008946-file004.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4339477