Recurrent H-bond graph motifs between metal tris-ethylenediamine cations and uncoordinated oxalate anions: Fitting a three pin plug into a two pin socket
Keene, Tony D.; Hursthouse, Michael B.; Price, Daniel J.; CrystEngComm 14 (2012) 116–; doi:10.1039/c1ce05837a

data_7207031
_publ_section_title
;
 Recurrent H-bond graph motifs between metal tris-ethylenediamine cations
 and uncoordinated oxalate anions: Fitting a three pin plug into a two pin
 socket
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              116
_journal_paper_doi               10.1039/c1ce05837a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         '2(C6 H24 Co N6), 3(C2 O4), 7(H2 O)'
_chemical_formula_sum            'C18 H62 Co2 N12 O19'
_chemical_formula_weight         868.66
_chemical_melting_point          ?
_chemical_name_common
;di-(tris-(ethylenediamine-N,N')-cobalt(iii)) tris-oxalate.
3.5 H2O
;
_chemical_name_systematic
;
di-[tris-(ethylenediamine-N,N')-cobalt(III)] tris-
oxalate. 3.5 H2O
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.446(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.964(2)
_cell_length_b                   10.3615(5)
_cell_length_c                   12.7579(8)
_cell_measurement_reflns_used    6385
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3485.5(4)
_computing_cell_refinement
'DENZO (Otwinowski and Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_collection       'DENZO (Otwinowski and Minor, 1997)'
_computing_data_reduction
'DENZO (Otwinowski and Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_molecular_graphics    'Diamond 3.2e (Brandenburg, 2010)'
_computing_structure_refinement
;SHELXS-97 (Sheldrick, 1997a) in WINGX (L.J. Farrugia, J. Appl. Cryst.,
1999, 32, 837-838
;
_computing_structure_solution
;SIR 92 (Altomore, Cascarno, Giacovazzo and Gualardi, 1993) in WINGX
(L.J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius Kappa CCD Area Detector'
_diffrn_measurement_method       '\f and \w scans to fill Ewald Sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1440
_diffrn_reflns_av_sigmaI/netI    0.1148
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12762
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  1.46882
_exptl_absorpt_correction_T_min  0.72583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3970
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+6.4301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1759
_reflns_number_gt                2516
_reflns_number_total             3970
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05837a.txt
_cod_data_source_block           en4_x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'N/A' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3485.6(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7207031