Synthesis of zinc trisubstituted hydrazido complexes and ortho-metalation of 4-(dimethylamino)pyridine.
Javed, Saba; Hoffman, David M.; Dalton transactions (Cambridge, England : 2003) 39 (2010) 11439–11444; doi:10.1039/c0dt00847h

data_7026889
_publ_section_title
;
 Synthesis of zinc trisubstituted hydrazido complexes and ortho-metalation
 of 4-(dimethylamino)pyridine.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11439
_journal_page_last               11444
_journal_paper_doi               10.1039/c0dt00847h
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C28 H54 N8 Zn3, C4 H10 O'
_chemical_formula_sum            'C32 H64 N8 O Zn3'
_chemical_formula_weight         773.02
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.337(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.5861(11)
_cell_length_b                   12.0656(4)
_cell_length_c                   27.1240(10)
_cell_measurement_reflns_used    8163
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      25.04
_cell_measurement_theta_min      1.73
_cell_volume                     7721.4(5)
_computing_cell_refinement       'SAINT v7.12A (Bruker-Nonius, 2004)'
_computing_data_collection       'APEX2 v1.0-27 (Bruker-Nonius, 2005)'
_computing_data_reduction        'SAINT v7.12A (Bruker-Nonius, 2004)'
_computing_structure_refinement  'SHELXL v5.10 (G.M. Sheldrick, 1997)'
_computing_structure_solution    'SHELXS v5.10 (G.M. Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 4K
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-Nonius APEX II CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0166
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19494
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    1.883
_exptl_absorpt_correction_T_max  0.9678
_exptl_absorpt_correction_T_min  0.6676
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Diamond plate'
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6824
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0.101
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+7.6584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                5374
_reflns_number_total             7176
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            c0dt00847h.txt
_cod_data_source_block           k1047[ZnEt2(iPrNNMe2)2(dmap)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        7721.3(5)
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               7026889