3-(4-Pyridyl)-acetylacetone ‒ a fully featured substituted pyridine and a flexible linker for complex materials
Merkens, Carina; Truong, Khai-Nghi; Englert, Ulli; Acta Crystallographica Section B 70 (2014) 705–713; doi:10.1107/S2052520614006210

data_2105949
_publ_section_title
;
 3-(4-Pyridyl)-acetylacetone -- a fully featured substituted pyridine and
 a flexible linker for complex materials
;
_journal_coeditor_code           BM5063
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              705
_journal_page_last               713
_journal_paper_doi               10.1107/S2052520614006210
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety
'C60 H60 Cd Cl2 Fe2 N6 O12, 6(C H4 O), 6(H2 O)'
_chemical_formula_sum            'C66 H96 Cd Cl2 Fe2 N6 O24'
_chemical_formula_weight         1652.50
_chemical_name_common            4
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                91.809(2)
_cell_angle_beta                 109.675(2)
_cell_angle_gamma                104.825(2)
_cell_formula_units_Z            1
_cell_length_a                   12.1351(13)
_cell_length_b                   13.2343(14)
_cell_length_c                   13.8728(15)
_cell_measurement_reflns_used    4039
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.32
_cell_volume                     2011.0(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXL-97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24575
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.610
_diffrn_reflns_theta_min         2.083
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.919
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         8416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+4.8255P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1303
_reflns_number_gt                6746
_reflns_number_total             8416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bm5063sup1.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C66 H96 Cd Cl2 Fe2 N6 O24 '
_cod_database_code               2105949
_cod_database_fobs_code          2105949
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.942
_shelx_hkl_checksum              11175
_shelx_res_checksum              83221
_shelxl_version_number           20.13