Nitrogen versus oxygen co-ordination of carboxamide-functionalized triazacyclononane ligands in transition metal ion complexes
Weyhermüller, Thomas; Weighardt, Karl; Chaudhuri, Phalguni; Journal of the Chemical Society, Dalton Transactions  (1998) 3805–; doi:10.1039/a806466k

data_7027067
_publ_section_title
;
 Nitrogen versus oxygen co-ordination of carboxamide-functionalized
 triazacyclononane ligands in transition metal ion complexes
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3805
_journal_paper_doi               10.1039/a806466k
_journal_year                    1998
_chemical_formula_structural     '[C12 H24 Cl N6 O3 V]2+, 2 (ClO4)-, 2 MeOH'
_chemical_formula_sum            'C14 H32 Cl3 N6 O13 V'
_chemical_formula_weight         649.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.284(3)
_cell_length_b                   11.925(3)
_cell_length_c                   32.508(6)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    100(2)
_cell_volume                     5150(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Siemens SMART CCD-Detector'
_diffrn_measurement_method       '\w-scan, 0.3 deg./frame'
_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  0.0989
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            44301
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.770
_exptl_absorpt_correction_type   'SADABS, G. Sheldrick 1994'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.147
_refine_ls_goodness_of_fit_obs   1.175
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         5726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_obs          0.0528
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+9.8247P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1381
_refine_ls_wR_factor_obs         0.1319
_reflns_number_observed          5261
_reflns_number_total             5865
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806466Ksup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0589P)^2^+9.8247P] 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^)+(0.0589P)^2^+9.8247P] 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        5149.7(20)
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7027067