Synthesis, Structure, and Preparative Transamination of Tetrazinc Carbamato Complexes Having the Basic Zinc Carboxylate Structure
C. Shawn McCowan; Thomas L. Groy; M. Tyler Caudle; Inorganic Chemistry 41 (2002) 1120–1127; doi:10.1021/ic010885v

data_4317624
_publ_section_title
;
 Synthesis, Structure, and Preparative Transamination of Tetrazinc
 Carbamato Complexes Having the Basic Zinc Carboxylate Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1120
_journal_page_last               1127
_journal_paper_doi               10.1021/ic010885v
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C32 H51 N7 O13 Zn4'
_chemical_formula_weight         1003.28
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                81.9070(10)
_cell_angle_beta                 75.4880(10)
_cell_angle_gamma                81.6540(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3178(6)
_cell_length_b                   10.6962(6)
_cell_length_c                   19.5130(11)
_cell_measurement_reflns_used    6341
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.54
_cell_volume                     2050.4(2)
_computing_cell_refinement       'Bruker SAINT ver. 6.02A'
_computing_data_collection       'Bruker SMART ver. 5.622'
_computing_data_reduction        'Bruker SAINT ver. 6.02A'
_computing_molecular_graphics    'Bruker SHELXTL ver. 5.1'
_computing_publication_material  'Bruker SHELXTL ver. 5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\w scan'
_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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16747
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.380
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         7241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0728
_reflns_number_gt                6141
_reflns_number_total             7241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010885v_1.cif
_cod_data_source_block           Zn_py_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317624