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_7027070
_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     '[C15 H30 Cr N6 O3]3+, 3 (ClO4)-, 3.5 H2O'
_chemical_formula_sum            'C15 H37 Cl3 Cr N6 O18.5'
_chemical_formula_weight         755.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 94.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.058(5)
_cell_length_b                   13.680(3)
_cell_length_c                   15.286(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    100(2)
_cell_volume                     6059(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  0.0523
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27201
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   'SADABS, G. Sheldrick 1994'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       'transparent prism'
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.422
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.126
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.103
_refine_ls_restrained_S_obs      1.126
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_obs          0.0738
_refine_ls_shift/esd_max         -0.032
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+23.9551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2378
_refine_ls_wR_factor_obs         0.1977
_reflns_number_observed          4615
_reflns_number_total             6826
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            806466Ksup1.cif
_cod_data_source_block           5
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1172P)^2^+23.9551P] 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^)+(0.1172P)^2^+23.9551P] 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      C2/c
_cod_original_formula_sum        'C15 H37 Cl3 Cr N6 O18.50'
_cod_database_code               7027070