Internal hydrogen bonding and amide co-ordination in zinc(II) complexes of a tripodal N4 ligand: structural, spectroscopic and reactivity studies
Juan C. Mareque Rivas; Rafael Torres Martín de Rosales; Simon Parsons; Dalton Trans.  (2003) 2156–2163; doi:10.1039/b301651j

data_7012828
_publ_section_title
;
 Internal hydrogen bonding and amide co-ordination in zinc(II)
 complexes of a tripodal N4 ligand: structural, spectroscopic and
 reactivity studies
;
_journal_issue                   11
_journal_name_full               'Dalton Trans.'
_journal_page_first              2156
_journal_page_last               2163
_journal_paper_doi               10.1039/b301651j
_journal_year                    2003
_chemical_formula_moiety         '[Zn(L1)][PF6}2.0.5MeOH'
_chemical_formula_sum            'C23.5 H29 F12 N5 O1.5 P2 Zn'
_chemical_formula_weight         760.83
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 106.072(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.424(2)
_cell_length_b                   11.3946(19)
_cell_length_c                   19.420(2)
_cell_measurement_reflns_used    62
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      25
_cell_volume                     3067.0(8)
_computing_cell_refinement       DIF4
_computing_data_collection       DIF4
_computing_data_reduction        REDU4
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Stoe Stadi-4 diffractometer'
_diffrn_measurement_method       0mega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7387
_diffrn_reflns_theta_full        70.09
_diffrn_reflns_theta_max         70.09
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.062
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.373
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
A numerical correction was applied by Gaussian integration following
refinement of the crystal face indices and dimensions against a 
set of psi-scans (Stoe X-Shape).
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       0.00023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         5451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+1.1969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0770
_reflns_number_gt                4514
_reflns_number_total             5451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301651j.txt
_cod_data_source_block           znrr26
_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 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Integration' changed
to 'integration' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C23.50 H29 F12 N5 O1.50 P2 Zn'
_cod_database_code               7012828