Synthesis and characterization of calcium beta-diketonate complexes. X-ray crystal and molecular structures of: [{Ca(tmhd)2}2(18-crown-6)], [Ca(dpp)2(thf)2] and [Ca(dpp)2(triglyme)].
El Habra, Naida; Benetollo, Franco; Casarin, Maurizio; Bolzan, Marco; Sartori, Andrea; Rossetto, Gilberto; Dalton transactions (Cambridge, England : 2003) 39 (2010) 8064–8070; doi:10.1039/c001854f

data_7025576
_publ_section_title
;
 Synthesis and characterization of calcium beta-diketonate complexes.
 X-ray crystal and molecular structures of: [{Ca(tmhd)2}2(18-crown-6)],
 [Ca(dpp)2(thf)2] and [Ca(dpp)2(triglyme)].
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8064
_journal_page_last               8070
_journal_paper_doi               10.1039/c001854f
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         '[(Ca(tmhd)~2~)~2~(18-crown-6)]'
_chemical_formula_sum            'C56 H100 Ca2 O14'
_chemical_formula_weight         1077.52
_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                72.84(3)
_cell_angle_beta                 80.19(3)
_cell_angle_gamma                72.33(3)
_cell_formula_units_Z            1
_cell_length_a                   10.558(2)
_cell_length_b                   10.574(2)
_cell_length_c                   15.776(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1597.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al. 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  ' Philips PW1100 '
_diffrn_measurement_method       \Q/2\Q
_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  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7307
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.9099
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'A. T. C. North, et al. Acta Crystallogr., A24 (1968) 351'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         6931
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.8482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                6301
_reflns_number_total             6931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001854f.txt
_cod_data_source_block           new-crown1
_cod_original_cell_volume        1597.1(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025576