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_7031162
_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(tachpyr)]Cl~2~ [CH~3~OH]'
_chemical_formula_sum            'C25 H34 Cl2 N6 Ni O'
_chemical_formula_weight         564.19
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.3180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4103(2)
_cell_length_b                   14.5893(3)
_cell_length_c                   19.1238(4)
_cell_measurement_reflns_used    6944
_cell_measurement_temperature    173(2)
_cell_volume                     2618.05(9)
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10411
_diffrn_reflns_theta_max         23.30
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.418
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.101
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_hydrogen_treatment    calc
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_obs          0.0581
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1086P)^2^+ 9.3599P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1938
_refine_ls_wR_factor_obs         0.1849
_reflns_number_observed          3496
_reflns_number_total             3757
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b209228j.txt
_cod_data_source_block           rp3
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-07-12

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(0.1086P)^2^+ 9.3599P] 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^)+(0.1086P)^2^+ 9.3599P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7031162