Solvothermal Synthesis of Oxamate-Based Helicate: Temperature Dependence of the Hydrogen Bond Structuring in the Solid
Lisnard, Laurent; Chamoreau, Lise-Marie; Li, Yanling; Journaux, Yves; Crystal Growth & Design 12 (2012) 4955–; doi:10.1021/cg300877r

data_4506797
_publ_section_title
;
 Solvothermal Synthesis of Oxamate-Based Helicate: Temperature Dependence
 of the Hydrogen Bond Structuring in the Solid
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4955
_journal_paper_doi               10.1021/cg300877r
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety
'C30 H18 Co2 N6 O18, 2(C6 H16 N), 3(C3 H7 N O), 10 (H2 O)'
_chemical_formula_sum            'C51 H91 Co2 N11 O31'
_chemical_formula_weight         1472.21
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.527(2)
_cell_length_b                   17.527(2)
_cell_length_c                   46.452(7)
_cell_measurement_reflns_used    94
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      18.8
_cell_measurement_theta_min      3.7
_cell_volume                     12358(3)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_molecular_graphics    'DIAMOND. Crystal Impact GbR, Bonn, Germany'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f and \w 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  0.0960
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            19834
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS, Bruker AXS Inc., Madison, 
Wisconsin, USA. 
;
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.828
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2416
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0849
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2619
_refine_ls_wR_factor_ref         0.2981
_reflns_number_gt                1595
_reflns_number_total             2416
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg300877r_si_003.cif
_cod_data_source_block           ll-st28d
_cod_original_cell_volume        12359(3)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4506797