A New Bridging Chelating Ligand for Crystal Engineering: Synthesis, Polymorphism, and Two Modes of Assembly of 1,4-Bis(3-phenyl-1,3-propanedion)benzene with Metal Cations Resulting in Either Discrete or Polymeric Complexes
Soldatov, D. V.; Zanina, A. S.; Enright, G. D.; Ratcliffe, C. I.; Ripmeester, J. A.; Crystal Growth & Design 3 (2003) 1005–; doi:10.1021/cg030016b

data_4505681
_publ_section_title
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 A New Bridging Chelating Ligand for Crystal Engineering:&#x2009;
 Synthesis, Polymorphism, and Two Modes of Assembly of
 1,4-Bis(3-phenyl-1,3-propanedion)benzene with Metal Cations Resulting in
 Either Discrete or Polymeric Complexes
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1005
_journal_paper_doi               10.1021/cg030016b
_journal_volume                  3
_journal_year                    2003
_chemical_formula_moiety         '[Ni3Py6L3]*4.68(CHCl3)'
_chemical_formula_sum            'C106.68 H82.68 Cl14.04 N6 Ni3 O12'
_chemical_formula_weight         2314.48
_chemical_name_systematic
; 
 Tris(mu!2$-(1,4-bis(3-phenyl-1,3-propanediono)benzene))-hexapyridine-tri-nickel(II), clathrate with Chloroform (1:4.68)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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                   24.640(4)
_cell_length_b                   24.640(4)
_cell_length_c                   30.549(5)
_cell_measurement_reflns_used    'all data'
_cell_measurement_temperature    173(2)
_cell_volume                     16062(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart CCD'
_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  0.0837
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            68100
_diffrn_reflns_theta_full        29.65
_diffrn_reflns_theta_max         29.65
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.9350
_exptl_absorpt_correction_T_min  0.7900
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             7101
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.763
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         10038
_refine_ls_number_restraints     1039
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                5043
_reflns_number_total             10038
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg030016b_s7.cif
_cod_data_source_block           nitk
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0909P)^2^+0.0000P] 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^)+(0.0909P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4505681