#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/55/7025578.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7025578
loop_
_publ_author_name
'El Habra, Naida'
'Benetollo, Franco'
'Casarin, Maurizio'
'Bolzan, Marco'
'Sartori, Andrea'
'Rossetto, Gilberto'
_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~(triglyme)]^.^0.25CH~2~Cl~2~'
_chemical_formula_sum            'C38.25 H40.5 Ca Cl0.5 O8'
_chemical_formula_weight         686.01
_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                 111.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.321(3)
_cell_length_b                   26.791(3)
_cell_length_c                   12.451(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3835.4(16)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  ' Philips PW1100 '
_diffrn_measurement_method       Θ/2Θ
_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  0.0136
_diffrn_reflns_av_sigmaI/netI    0.0568
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7043
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.8083
_exptl_absorpt_correction_T_min  0.4268
_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    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1450
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         6716
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0889
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1786P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1946
_refine_ls_wR_factor_ref         0.2052
_reflns_number_gt                3286
_reflns_number_total             6716
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c001854f.txt
_cod_data_source_block           ca-triglyme
_cod_original_cell_volume        3835.4(14)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C38.25 H40.50 Ca Cl0.50 O8'
_cod_database_code               7025578
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ca Ca 0.91436(9) 0.13334(4) 0.56620(10) 0.0582(4) Uani 1 1 d .
O1 O 1.0963(3) 0.10004(15) 0.6798(3) 0.0709(11) Uani 1 1 d .
O2 O 1.0250(3) 0.12436(16) 0.4465(3) 0.0708(11) Uani 1 1 d .
O3 O 0.8857(3) 0.11193(16) 0.7418(3) 0.0724(11) Uani 1 1 d .
O7 O 0.7685(4) 0.12184(18) 0.3562(4) 0.0851(13) Uani 1 1 d .
O5 O 1.0254(5) 0.20992(19) 0.6544(6) 0.1155(19) Uani 1 1 d .
O6 O 0.8727(6) 0.21143(19) 0.4361(5) 0.1084(17) Uani 1 1 d .
O4 O 0.7443(4) 0.17348(17) 0.5666(4) 0.0815(13) Uani 1 1 d .
O8 O 0.8316(4) 0.05012(16) 0.5178(4) 0.0839(13) Uani 1 1 d .
C1 C 1.1953(5) 0.10293(19) 0.6742(5) 0.0553(14) Uani 1 1 d .
C2 C 1.2196(5) 0.1160(2) 0.5762(5) 0.0613(15) Uani 1 1 d .
H2 H 1.2970 0.1191 0.5833 0.074 Uiso 1 1 calc R
C3 C 1.1330(5) 0.12485(19) 0.4672(5) 0.0576(14) Uani 1 1 d .
C4 C 1.1708(5) 0.13275(19) 0.3657(5) 0.0587(14) Uani 1 1 d .
C5 C 1.2730(5) 0.1556(2) 0.3744(6) 0.0747(17) Uani 1 1 d .
H5 H 1.3229 0.1671 0.4454 0.090 Uiso 1 1 calc R
C6 C 1.3024(7) 0.1617(3) 0.2782(7) 0.091(2) Uani 1 1 d .
H6 H 1.3708 0.1781 0.2841 0.110 Uiso 1 1 calc R
C7 C 1.2308(8) 0.1437(3) 0.1743(7) 0.100(3) Uani 1 1 d .
H7 H 1.2515 0.1476 0.1099 0.120 Uiso 1 1 calc R
C8 C 1.1290(7) 0.1200(3) 0.1638(6) 0.0840(19) Uani 1 1 d .
H8 H 1.0805 0.1076 0.0930 0.101 Uiso 1 1 calc R
C9 C 1.1004(6) 0.1150(2) 0.2590(5) 0.0739(17) Uani 1 1 d .
H9 H 1.0312 0.0991 0.2522 0.089 Uiso 1 1 calc R
C10 C 1.2949(5) 0.0888(2) 0.7827(5) 0.0616(15) Uani 1 1 d .
C11 C 1.4074(5) 0.0803(3) 0.7853(6) 0.0835(19) Uani 1 1 d .
H11 H 1.4237 0.0837 0.7183 0.100 Uiso 1 1 calc R
C12 C 1.4959(6) 0.0667(3) 0.8880(7) 0.098(2) Uani 1 1 d .
H12 H 1.5698 0.0602 0.8873 0.117 Uiso 1 1 calc R
C13 C 1.4776(7) 0.0628(3) 0.9866(6) 0.088(2) Uani 1 1 d .
H13 H 1.5387 0.0550 1.0543 0.106 Uiso 1 1 calc R
C14 C 1.3662(8) 0.0705(3) 0.9874(6) 0.098(2) Uani 1 1 d .
H14 H 1.3512 0.0665 1.0550 0.117 Uiso 1 1 calc R
C15 C 1.2760(6) 0.0845(2) 0.8841(6) 0.0777(18) Uani 1 1 d .
H15 H 1.2023 0.0910 0.8852 0.093 Uiso 1 1 calc R
C16 C 0.8151(5) 0.1237(2) 0.7874(5) 0.0597(14) Uani 1 1 d .
C17 C 0.7224(5) 0.1569(2) 0.7421(5) 0.0650(15) Uani 1 1 d .
H17 H 0.6775 0.1642 0.7863 0.078 Uiso 1 1 calc R
C18 C 0.6936(5) 0.1793(2) 0.6371(5) 0.0632(15) Uani 1 1 d .
C19 C 0.5883(5) 0.2158(2) 0.5967(5) 0.0637(15) Uani 1 1 d .
C20 C 0.5832(7) 0.2504(2) 0.5119(6) 0.0852(19) Uani 1 1 d .
H20 H 0.6416 0.2508 0.4811 0.102 Uiso 1 1 calc R
C21 C 0.4939(8) 0.2839(3) 0.4729(7) 0.111(3) Uani 1 1 d .
H21 H 0.4904 0.3061 0.4144 0.133 Uiso 1 1 calc R
C22 C 0.4114(8) 0.2845(3) 0.5197(8) 0.117(3) Uani 1 1 d .
H22 H 0.3527 0.3084 0.4964 0.141 Uiso 1 1 calc R
C23 C 0.4135(6) 0.2499(3) 0.6024(7) 0.101(3) Uani 1 1 d .
H23 H 0.3539 0.2493 0.6317 0.122 Uiso 1 1 calc R
C24 C 0.5032(5) 0.2163(2) 0.6415(6) 0.0776(18) Uani 1 1 d .
H24 H 0.5056 0.1938 0.6991 0.093 Uiso 1 1 calc R
C25 C 0.8256(5) 0.0958(2) 0.8970(5) 0.0620(15) Uani 1 1 d .
C26 C 0.8609(6) 0.0472(3) 0.9103(5) 0.0785(18) Uani 1 1 d .
H26 H 0.8856 0.0328 0.8551 0.094 Uiso 1 1 calc R
C27 C 0.8612(7) 0.0186(3) 1.0035(6) 0.090(2) Uani 1 1 d .
H27 H 0.8783 -0.0153 1.0063 0.108 Uiso 1 1 calc R
C28 C 0.8365(6) 0.0401(4) 1.0899(6) 0.097(2) Uani 1 1 d .
H28 H 0.8432 0.0218 1.1554 0.116 Uiso 1 1 calc R
C29 C 0.8011(6) 0.0899(3) 1.0812(6) 0.085(2) Uani 1 1 d .
H29 H 0.7813 0.1047 1.1394 0.102 Uiso 1 1 calc R
C30 C 0.7957(5) 0.1171(3) 0.9848(6) 0.0810(19) Uani 1 1 d .
H30 H 0.7716 0.1502 0.9784 0.097 Uiso 1 1 calc R
C31 C 1.1052(10) 0.2131(4) 0.7645(10) 0.155(4) Uani 1 1 d .
H31A H 1.1820 0.2156 0.7621 0.186 Uiso 1 1 calc R
H31B H 1.1002 0.1838 0.8069 0.186 Uiso 1 1 calc R
H31C H 1.0892 0.2422 0.8015 0.186 Uiso 1 1 calc R
C32 C 1.0057(11) 0.2554(4) 0.5953(13) 0.161(5) Uani 1 1 d .
H32A H 1.0785 0.2736 0.6160 0.193 Uiso 1 1 calc R
H32B H 0.9521 0.2753 0.6185 0.193 Uiso 1 1 calc R
C33 C 0.9584(11) 0.2485(4) 0.4720(15) 0.181(6) Uani 1 1 d .
H33A H 0.9253 0.2798 0.4360 0.218 Uiso 1 1 calc R
H33B H 1.0211 0.2398 0.4457 0.218 Uiso 1 1 calc R
C34 C 0.8214(9) 0.2024(3) 0.3161(8) 0.116(3) Uani 1 1 d .
H34A H 0.8767 0.1867 0.2875 0.139 Uiso 1 1 calc R
H34B H 0.7944 0.2333 0.2744 0.139 Uiso 1 1 calc R
C35 C 0.7213(8) 0.1680(4) 0.3036(6) 0.119(3) Uani 1 1 d .
H35A H 0.6717 0.1823 0.3410 0.143 Uiso 1 1 calc R
H35B H 0.6753 0.1630 0.2229 0.143 Uiso 1 1 calc R
C36 C 0.6874(7) 0.0862(4) 0.3539(7) 0.112(3) Uani 1 1 d .
H36A H 0.6356 0.0803 0.2754 0.134 Uiso 1 1 calc R
H36B H 0.6412 0.0975 0.3981 0.134 Uiso 1 1 calc R
C37 C 0.7523(8) 0.0379(3) 0.4062(7) 0.103(3) Uani 1 1 d .
H37A H 0.6978 0.0127 0.4111 0.124 Uiso 1 1 calc R
H37B H 0.7937 0.0251 0.3589 0.124 Uiso 1 1 calc R
C38 C 0.8856(8) 0.0076(3) 0.5842(8) 0.115(3) Uani 1 1 d .
H38A H 0.8273 -0.0135 0.5948 0.138 Uiso 1 1 calc R
H38B H 0.9389 0.0183 0.6579 0.138 Uiso 1 1 calc R
H38C H 0.9271 -0.0106 0.5448 0.138 Uiso 1 1 calc R
C39 C 0.4883(12) 0.0478(5) 0.4947(12) 0.037(3) Uiso 0.25 1 d PD
Cl1 Cl 0.397(2) 0.0261(11) 0.3551(15) 0.184(10) Uiso 0.25 1 d PD
Cl2 Cl 0.5841(19) 0.0170(9) 0.6163(16) 0.174(10) Uiso 0.25 1 d PD
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Ca O4 145.79(15) . .
O1 Ca O2 72.55(13) . .
O4 Ca O2 139.62(15) . .
O1 Ca O3 77.46(14) . .
O4 Ca O3 71.68(14) . .
O2 Ca O3 148.67(15) . .
O1 Ca O8 91.46(16) . .
O4 Ca O8 97.15(17) . .
O2 Ca O8 92.06(15) . .
O3 Ca O8 79.71(15) . .
O1 Ca O5 78.10(17) . .
O4 Ca O5 88.34(18) . .
O2 Ca O5 90.69(19) . .
O3 Ca O5 91.86(19) . .
O8 Ca O5 167.9(2) . .
O1 Ca O6 128.00(18) . .
O4 Ca O6 69.82(17) . .
O2 Ca O6 73.56(17) . .
O3 Ca O6 134.60(17) . .
O8 Ca O6 128.0(2) . .
O5 Ca O6 64.1(2) . .
O1 Ca O7 136.27(15) . .
O4 Ca O7 76.30(15) . .
O2 Ca O7 72.62(14) . .
O3 Ca O7 127.63(15) . .
O8 Ca O7 64.33(16) . .
O5 Ca O7 127.7(2) . .
O6 Ca O7 63.65(19) . .
C1 O1 Ca 133.0(4) . .
C3 O2 Ca 132.4(4) . .
C16 O3 Ca 135.4(4) . .
C36 O7 C35 114.8(7) . .
C36 O7 Ca 109.7(4) . .
C35 O7 Ca 112.3(5) . .
C31 O5 C32 113.4(8) . .
C31 O5 Ca 125.1(6) . .
C32 O5 Ca 121.4(6) . .
C33 O6 C34 117.2(9) . .
C33 O6 Ca 114.6(6) . .
C34 O6 Ca 115.8(5) . .
C18 O4 Ca 136.4(4) . .
C37 O8 C38 113.5(6) . .
C37 O8 Ca 122.2(4) . .
C38 O8 Ca 121.4(5) . .
O1 C1 C2 125.6(5) . .
O1 C1 C10 115.6(5) . .
C2 C1 C10 118.8(5) . .
C1 C2 C3 123.7(5) . .
O2 C3 C2 124.9(5) . .
O2 C3 C4 116.7(5) . .
C2 C3 C4 118.3(5) . .
C5 C4 C9 118.0(6) . .
C5 C4 C3 123.3(5) . .
C9 C4 C3 118.7(5) . .
C4 C5 C6 120.4(6) . .
C7 C6 C5 119.9(7) . .
C6 C7 C8 120.8(7) . .
C9 C8 C7 118.5(7) . .
C8 C9 C4 122.3(6) . .
C15 C10 C11 117.5(6) . .
C15 C10 C1 119.5(5) . .
C11 C10 C1 122.9(5) . .
C10 C11 C12 120.4(7) . .
C13 C12 C11 122.0(7) . .
C12 C13 C14 119.3(7) . .
C13 C14 C15 119.1(7) . .
C10 C15 C14 121.5(7) . .
O3 C16 C17 125.8(6) . .
O3 C16 C25 116.0(5) . .
C17 C16 C25 118.0(5) . .
C18 C17 C16 124.1(5) . .
O4 C18 C17 126.2(5) . .
O4 C18 C19 114.7(5) . .
C17 C18 C19 119.1(5) . .
C24 C19 C20 118.4(6) . .
C24 C19 C18 123.5(6) . .
C20 C19 C18 118.0(6) . .
C21 C20 C19 121.3(7) . .
C22 C21 C20 119.5(8) . .
C21 C22 C23 120.1(7) . .
C24 C23 C22 120.1(8) . .
C19 C24 C23 120.4(7) . .
C26 C25 C30 117.3(6) . .
C26 C25 C16 119.9(5) . .
C30 C25 C16 122.7(6) . .
C25 C26 C27 122.2(6) . .
C28 C27 C26 119.7(7) . .
C27 C28 C29 120.1(7) . .
C30 C29 C28 119.0(7) . .
C29 C30 C25 121.4(7) . .
O5 C32 C33 112.0(9) . .
O6 C33 C32 113.6(11) . .
O6 C34 C35 104.6(7) . .
O7 C35 C34 107.5(6) . .
O7 C36 C37 108.2(6) . .
O8 C37 C36 106.9(6) . .
Cl2 C39 Cl1 132.6(14) . .
Cl2 C39 Cl2 99.5(12) . 3_656
Cl1 C39 Cl2 33.3(9) . 3_656
Cl2 Cl1 C39 92.1(18) 3_656 .
Cl1 Cl2 C39 135(2) 3_656 .
Cl1 Cl2 C39 54.6(13) 3_656 3_656
C39 Cl2 C39 80.5(11) . 3_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca O1 2.354(4) .
Ca O4 2.357(4) .
Ca O2 2.367(4) .
Ca O3 2.406(4) .
Ca O8 2.436(4) .
Ca O5 2.492(5) .
Ca O6 2.582(5) .
Ca O7 2.605(5) .
O1 C1 1.249(6) .
O2 C3 1.260(6) .
O3 C16 1.238(6) .
O7 C36 1.375(8) .
O7 C35 1.423(9) .
O5 C31 1.373(10) .
O5 C32 1.399(11) .
O6 C33 1.400(12) .
O6 C34 1.418(10) .
O4 C18 1.256(7) .
O8 C37 1.420(9) .
O8 C38 1.424(8) .
C1 C2 1.402(7) .
C1 C10 1.511(8) .
C2 C3 1.413(8) .
C3 C4 1.511(8) .
C4 C5 1.370(8) .
C4 C9 1.384(8) .
C5 C6 1.380(9) .
C6 C7 1.365(10) .
C7 C8 1.369(10) .
C8 C9 1.360(9) .
C10 C15 1.369(8) .
C10 C11 1.393(8) .
C11 C12 1.398(9) .
C12 C13 1.329(10) .
C13 C14 1.392(10) .
C14 C15 1.415(10) .
C16 C17 1.396(8) .
C16 C25 1.521(8) .
C17 C18 1.365(8) .
C18 C19 1.557(8) .
C19 C24 1.353(8) .
C19 C20 1.389(8) .
C20 C21 1.367(9) .
C21 C22 1.342(11) .
C22 C23 1.380(11) .
C23 C24 1.370(9) .
C25 C26 1.362(9) .
C25 C30 1.394(8) .
C26 C27 1.391(9) .
C27 C28 1.347(10) .
C28 C29 1.396(10) .
C29 C30 1.385(9) .
C32 C33 1.444(15) .
C34 C35 1.501(12) .
C36 C37 1.538(12) .
C39 Cl2 1.757(10) .
C39 Cl1 1.794(10) .
C39 Cl2 2.20(3) 3_656
Cl1 Cl2 1.21(3) 3_656
Cl2 Cl1 1.21(3) 3_656
Cl2 C39 2.20(3) 3_656
