Synchrotron X-ray Charge Density Study of Coordination Polymer Co~3~(C~8~H~4~O~4~)~4~(C~4~H~12~N)~2~(C~5~H~11~NO)~3~ at 16 K
H. F. Clausen; J. Overgaard; Yu-Sheng Chen; Bo Brummerstedt Iversen; Journal of the American Chemical Society 130 (2008) 7988–7996; doi:10.1021/ja8007215

data_4107917
_publ_contact_author_address
;University of Aarhus
Department of Chemistry
Laboratory of Inorganic Chemistry
Langelandsgade 140
DK-8000 Aarhus C
Denmark
;
_publ_contact_author_email       bo@chem.au.dk
_publ_contact_author_fax         '+458619 6199'
_publ_contact_author_name        'Bo Brummerstedt Iversen'
_publ_contact_author_phone       +4589423969
_publ_section_title
;
 Synchrotron X-ray Charge Density Study of Coordination Polymer
 Co~3~(C~8~H~4~O~4~)~4~(C~4~H~12~N)~2~(C~5~H~11~NO)~3~ at 16 K
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7988
_journal_page_last               7996
_journal_paper_doi               10.1021/ja8007215
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety
'(Co 2+)3, (C8 H4 O4 2-)4 2-, 2(C5 H11 N O), 2(C4 H12 N O +), C5 H11 N O'
_chemical_formula_sum            'C55 H73 Co3 N5 O19'
_chemical_formula_weight         1284.98
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_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
_cell_angle_beta                 92.5200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.1947(16)
_cell_length_b                   9.7794(4)
_cell_length_c                   18.2274(7)
_cell_measurement_reflns_used    9009
_cell_measurement_temperature    16(2)
_cell_measurement_theta_max      30.686
_cell_measurement_theta_min      2.276
_cell_volume                     5911.3(4)
_computing_cell_refinement       'SMART and SAINT (Bruker,1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'Koritsanszky et al, (2003)'
_computing_publication_material  'Koritsanszky et al, (2003)'
_computing_structure_refinement  'Koritsanszky et al, (2003)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      16(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.510
_diffrn_measured_fraction_theta_max 0.510
_diffrn_measurement_device_type  'APS,ChemMatCars, Huber type diffractometer'
_diffrn_measurement_method       \f-scans
_diffrn_radiation_monochromator  'diamond (111)'
_diffrn_radiation_source         'Advanced photon source'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       81
_diffrn_reflns_limit_h_min       -81
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            165663
_diffrn_reflns_theta_full        31.48
_diffrn_reflns_theta_max         31.48
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       plate
_exptl_crystal_F_000             2684
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.627
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     993
_refine_ls_number_reflns         18635
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.023
_refine_ls_R_Fsqd_factor         0.035
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;

calc w2 = 1/[s^2^(Fo^2^)]

;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.053
_reflns_number_gt                18635
_reflns_number_total             25472
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8007215-file004.cif
_cod_data_source_block           shelx3
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4107917