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_7025577
_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(dpp)~2~(thf)~2~]'
_chemical_formula_sum            'C38 H38 Ca O6'
_chemical_formula_weight         630.76
_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                 104.10(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.939(2)
_cell_length_b                   15.574(3)
_cell_length_c                   10.861(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1630.5(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3733
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.8466
_exptl_absorpt_correction_T_min  0.5138
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'A. T. C. North, et al. Acta Crystallogr., A24 (1968) 351'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.155
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                2002
_reflns_number_total             3546
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001854f.txt
_cod_data_source_block           ca-thf
_cod_original_cell_volume        1630.5(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7025577