New co-ordination compounds derived from barium(II) and the anionic 4-tert-butylacetyl-3-methyl-1-phenylpyrazol-5-onate ligand (Q−). Crystal and molecular structure of [Ba2Q4(H2O)4], [Ba2Q4(Him)4], [BaQ2(tetraglyme)] (tetraglyme = 2,5,8,11,14-pentaoxapentadecane) and [BaQ2(phen)2]
Pettinari, Claudio; Marchetti, Fabio; Cingolani, Augusto; Leonesi, Dante; Troyanov, Sergei; Drozdov, Andrei; Journal of the Chemical Society, Dalton Transactions  (1999) 1555–; doi:10.1039/a900463g

data_7027261
_publ_section_title
;
 New co-ordination compounds derived from barium(II) and the anionic
 4-tert-butylacetyl-3-methyl-1-phenylpyrazol-5-onate ligand (Q&#x2212;).
 Crystal and molecular structure of [Ba2Q4(H2O)4], [Ba2Q4(Him)4],
 [BaQ2(tetraglyme)]
 (tetraglyme&#x2005;=&#x2005;2,5,8,11,14-pentaoxapentadecane) and
 [BaQ2(phen)2]
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1555
_journal_paper_doi               10.1039/a900463g
_journal_year                    1999
_chemical_formula_sum            'C66 H86 Ba2 Cl6 N8 O12'
_chemical_formula_weight         1670.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.34(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.067(3)
_cell_length_b                   18.070(4)
_cell_length_c                   15.153(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      5
_cell_volume                     3656.1(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0753
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23947
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.295
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+12.5491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                5443
_reflns_number_total             6440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            900463gsup1.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+12.5491P] 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^)+(0.0468P)^2^+12.5491P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3656.1(13)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027261