Synthesis of two covalently linked bis(2,2':6',2″-terpyridine) (terpy) chelating ligands with different length spacers, comparison of the crystal structures of their mononuclear nickel(II) complexes, and kinetic and mechanistic studies of the reaction of one ligand with [Fe(terpy)2]2+
Priimov, Gleb U.; Moore, Peter; Maritim, Philip K.; Butalanyi, Pamela K.; Alcock, Nathaniel W.; Journal of the Chemical Society, Dalton Transactions  (2000) 445–; doi:10.1039/a907543g

data_7008967
_publ_section_title
;
 Synthesis of two covalently linked bis(2,2':6',2&#x2033;-terpyridine)
 (terpy) chelating ligands with different length spacers, comparison of
 the crystal structures of their mononuclear nickel(II) complexes, and
 kinetic and mechanistic studies of the reaction of one ligand with
 [Fe(terpy)2]2+
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              445
_journal_paper_doi               10.1039/a907543g
_journal_year                    2000
_chemical_formula_sum            'C38.5 H35 F12 N7 Ni O0.25 P2 S2'
_chemical_formula_weight         1012.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.8148(3)
_cell_length_b                   11.2892(2)
_cell_length_c                   14.9759(2)
_cell_measurement_reflns_used    6422
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      3
_cell_volume                     4533.47(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0541
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19958
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            golden-yellow
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         7019
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.741
_refine_ls_shift/su_mean         0.139
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+1.9161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1826
_reflns_number_gt                3998
_reflns_number_total             7019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a907543g.txt
_cod_data_source_block           pkb21
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (17
times).

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_original_formula_sum        'C38.50 H35 F12 N7 Ni O0.25 P2 S2'
_cod_database_code               7008967