Steric effects caused by N-alkylation of the tripodal chelator N,N′,N″-tris(2-pyridylmethyl)-cis,cis-1,3,5-triaminocyclohexane (tachpyr): structural and electronic properties of the Mn(ii), Co(ii), Ni(ii), Cu(ii) and Zn(ii) complexes
Park, Gyungse; Przyborowska, Ann M.; Ye, Neng; Tsoupas, Nicole M.; Bauer, Cary B.; Broker, Grant A.; Rogers, Robin D.; Brechbiel, Martin W.; Planalp, Roy P.; Dalton Transactions  (2003) 318–; doi:10.1039/b209228j

data_7031163
_publ_section_title
;
 Steric effects caused by N-alkylation of the tripodal chelator
 N,N&#x2032;,N&#x2033;-tris(2-pyridylmethyl)-cis,cis-1,3,5-triaminocyclohexane
 (tachpyr): structural and electronic properties of the Mn(ii), Co(ii),
 Ni(ii), Cu(ii) and Zn(ii) complexes
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              318
_journal_paper_doi               10.1039/b209228j
_journal_year                    2003
_chemical_formula_moiety         '[Ni(Me3tachpyr)][ClO~4~]~2~'
_chemical_formula_structural     'RP20 (NY1P182-2)'
_chemical_formula_sum            'C29 H39 Cl2 N7 Ni O8'
_chemical_formula_weight         743.28
_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
_cell_angle_alpha                75.553(1)
_cell_angle_beta                 86.028(1)
_cell_angle_gamma                61.606(1)
_cell_formula_units_Z            2
_cell_length_a                   9.9925(7)
_cell_length_b                   10.2145(7)
_cell_length_c                   18.1508(13)
_cell_measurement_reflns_used    3202
_cell_measurement_temperature    173(2)
_cell_volume                     1575.56(19)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10108
_diffrn_reflns_theta_max         27.90
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0013(6)
_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_all   1.051
_refine_ls_goodness_of_fit_obs   1.076
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.076
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_obs          0.0612
_refine_ls_shift/esd_max         -0.043
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+ 2.4430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1465
_refine_ls_wR_factor_obs         0.1125
_reflns_number_observed          4168
_reflns_number_total             7011
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b209228j.txt
_cod_data_source_block           rp20
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+ 2.4430P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+ 2.4430P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1575.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7031163