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_4339478
_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 O3 Zn, 2(Cl O4)'
_chemical_formula_sum            'C26 H34 Cl2 N6 O11 Zn'
_chemical_formula_weight         742.86
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2006-04-19T17:49:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                94.609(6)
_cell_angle_beta                 109.246(5)
_cell_angle_gamma                112.763(5)
_cell_formula_units_Z            2
_cell_length_a                   11.050(3)
_cell_length_b                   12.046(3)
_cell_length_c                   13.570(4)
_cell_measurement_reflns_used    799
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      21.405
_cell_measurement_theta_min      2.46
_cell_measurement_wavelength     0.71073
_cell_volume                     1527.0(7)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_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, Beurskens et al. 1999'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega 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  0.1087
_diffrn_reflns_av_unetI/netI     0.159
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15721
_diffrn_reflns_theta_full        25.81
_diffrn_reflns_theta_max         25.81
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    1.049
_exptl_absorpt_correction_T_max  0.9502
_exptl_absorpt_correction_T_min  0.5363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS: Area-Detector Absorption Correction;  
Siemens Industrial Automation, Inc.: Madison, WI, 1996. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.133
_refine_diff_density_min         -1.041
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5817
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1536
_refine_ls_R_factor_gt           0.0603
_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^)+(0.0600P)^2^+1.0802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1611
_reflns_number_gt                2960
_reflns_number_total             5817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic7008946-file004.cif
_cod_data_source_block           compound5
_cod_database_code               4339478