Synthesis and characterisation of zinc(ii) complexes of tripodal N7 ligands involving pyridine and amine or amide nitrogen donors. Crystal structure of a zinc(ii) complex
Mohamadou, Aminou; GÃ©rard, Christian; Journal of the Chemical Society, Dalton Transactions  (2001) 3320–; doi:10.1039/b104777a

data_7702654
_publ_section_title
;
 Synthesis and characterisation of zinc(ii) complexes of tripodal N7
 ligands involving pyridine and amine or amide nitrogen donors. Crystal
 structure of a zinc(ii) complex
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3320
_journal_paper_doi               10.1039/b104777a
_journal_year                    2001
_chemical_formula_moiety         'C24 H33 Cl2 N7 O8 Zn'
_chemical_formula_sum            'C24 H33 Cl2 N7 O8 Zn'
_chemical_formula_weight         683.85
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 103.543(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9115(2)
_cell_length_b                   16.1184(3)
_cell_length_c                   19.2407(5)
_cell_measurement_temperature    294
_cell_volume                     2988.38(13)
_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
;
12287 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance ==  35. mm.
Scan angle ==  2.0 deg 1 scans of   30 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   90 frames
Set 2 Theta ==   -5.90 Kappa == -164.00 Phi   ==    0.00   19 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       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12287
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  '? =='
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.52
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.505
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.485
_refine_ls_goodness_of_fit_ref   1.270
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     379
_refine_ls_number_reflns         3876
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.132
_refine_ls_wR_factor_ref         0.070
_reflns_number_gt                3876
_reflns_number_total             7072
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b104777a.txt
_cod_data_source_block           'global_for_complex_[ZnTPAA](ClO4)2_1.'
_cod_original_cell_volume        2988.4(1)
_cod_database_code               7702654