Five-coordinate nickel(II) complexes with carboxylate anions and derivatives of 1,5,9-triazacyclododec-1-ene: structural and 1H NMR spectroscopic studies.
Santana, M. Dolores; Lozano, A. Abel; Garcia, Gabriel; Lopez, Gregorio; Perez, Jose; Dalton transactions (Cambridge, England : 2003)  (2005) 104–109; doi:10.1039/b413547d

data_7000083
_publ_section_title
;
 Five-coordinate nickel(II) complexes with carboxylate anions and
 derivatives of 1,5,9-triazacyclododec-1-ene: structural and 1H NMR
 spectroscopic studies.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              104
_journal_page_last               109
_journal_paper_doi               10.1039/b413547d
_journal_year                    2005
_chemical_formula_moiety         'C22 H34 N3 Ni O4, F6 P, H2 O'
_chemical_formula_sum            'C22 H36 F6 N3 Ni O5 P'
_chemical_formula_weight         626.22
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.8200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2175(4)
_cell_length_b                   15.2313(8)
_cell_length_c                   10.7289(5)
_cell_measurement_reflns_used    6285
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.978
_cell_measurement_theta_min      2.508
_cell_volume                     1326.98(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker 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  0.0181
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15098
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.13
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.872
_exptl_absorpt_correction_T_max  0.8877
_exptl_absorpt_correction_T_min  0.7677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.519
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.038(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.9715P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                5813
_reflns_number_total             5943
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b413547d.txt
_cod_data_source_block           6
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_sg_symbol_H-M      P21
_cod_database_code               7000083