Copper and calcium complexes with the anionic O2-donor 4-tert-butylacetyl-3-methyl-1-phenylpyrazol-5-onato (Q−). Influence of hydrogen-bond interactions on lattice architecture in the crystal structures of [CuQ2(H2O)] and [CaQ2(EtOH)2]
Marchetti, Fabio; Pettinari, Claudio; Cingolani, Augusto; Leonesi, Dante; Drozdov, Andrei; Troyanov, Sergei I.; Journal of the Chemical Society, Dalton Transactions  (1998) 3325–; doi:10.1039/a804768e

data_7028046
_publ_section_title
;
 Copper and calcium complexes with the anionic O2-donor
 4-tert-butylacetyl-3-methyl-1-phenylpyrazol-5-onato (Q&#x2212;).
 Influence of hydrogen-bond interactions on lattice architecture in the
 crystal structures of [CuQ2(H2O)] and [CaQ2(EtOH)2]
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3325
_journal_paper_doi               10.1039/a804768e
_journal_year                    1998
_chemical_formula_sum            'C32 H40 Cu N4 O5'
_chemical_formula_weight         624.22
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.93(3)
_cell_angle_beta                 73.23(3)
_cell_angle_gamma                78.72(3)
_cell_formula_units_Z            2
_cell_length_a                   9.169(2)
_cell_length_b                   13.410(3)
_cell_length_c                   14.350(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      16
_cell_volume                     1536.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  STADI-4
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3744
_diffrn_reflns_theta_max         22.00
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0.02
_diffrn_standards_interval_time  2h
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0019(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+1.8697P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1392
_reflns_number_gt                3209
_reflns_number_total             3744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            e804768sup1.cif
_cod_data_source_block           CuQ2.H2O_Compound_No.1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.0731P)^2^+1.8697P] 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^)+(0.0731P)^2^+1.8697P] 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        1536.3(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7028046