#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:36:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179853 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/49/7014933.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_7014933
loop_
_publ_author_name
'Deacon, Glen B.'
'Junk, Peter C.'
'Urbatsch, Aron'
_publ_section_title
;
 Divalent metal complexes (Ca, Sr, Ba, Yb) of the unsymmetrical
 3-(2'-thienyl)-5-(trifluoromethyl)pyrazolate ligand.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1601
_journal_page_last               1609
_journal_paper_doi               10.1039/c0dt01289k
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety
;
C24 H28 Ca F6 N4 O4 S2
;
_chemical_formula_sum            'C24 H28 Ca F6 N4 O4 S2'
_chemical_formula_weight         654.70
_chemical_name_common            (Ca(ttfpz)2(dme)2)
_chemical_name_systematic
;
[Ca(ttfpz)2(dme)2]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 99.6190(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7619(2)
_cell_length_b                   18.9930(6)
_cell_length_c                   19.8639(7)
_cell_measurement_reflns_used    39058
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.14
_cell_volume                     2887.20(16)
_computing_cell_refinement       'Bruker SMART (Bruker)'
_computing_data_collection       'Bruker SMART (Bruker)'
_computing_data_reduction        'Bruker SAINT (Bruker)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39058
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.14
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.9575
_exptl_absorpt_correction_T_min  0.9174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.075
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0470
_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/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                5867
_reflns_number_total             6611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT01289K.TXT
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7014933
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.51741(5) 0.08112(2) 0.30344(2) 0.01349(11) Uani 1 1 d . . .
S1 S 0.33340(9) 0.25267(3) 0.44274(3) 0.02840(15) Uani 1 1 d . . .
S2 S 0.70124(9) 0.01533(3) 0.09993(3) 0.03067(16) Uani 1 1 d . . .
F1 F 0.2845(3) 0.29139(10) 0.09307(9) 0.0620(6) Uani 1 1 d . . .
F4 F 0.7983(4) -0.19630(9) 0.38794(10) 0.0665(7) Uani 1 1 d . . .
F2 F 0.1282(3) 0.19845(11) 0.09150(8) 0.0530(5) Uani 1 1 d . . .
F5 F 0.6194(3) -0.12384(14) 0.42040(10) 0.0714(7) Uani 1 1 d . . .
F3 F 0.4043(3) 0.18906(10) 0.09842(8) 0.0459(4) Uani 1 1 d . . .
F6 F 0.8885(3) -0.10214(11) 0.43813(9) 0.0576(5) Uani 1 1 d . . .
O1 O 0.6549(2) 0.11914(8) 0.41635(8) 0.0205(3) Uani 1 1 d . . .
O2 O 0.7862(2) 0.14728(8) 0.30394(8) 0.0201(3) Uani 1 1 d . . .
O3 O 0.2860(2) 0.01629(9) 0.23141(8) 0.0231(3) Uani 1 1 d . . .
O4 O 0.30905(19) 0.02655(8) 0.36954(8) 0.0193(3) Uani 1 1 d . . .
N1 N 0.3675(2) 0.19411(10) 0.30053(9) 0.0186(4) Uani 1 1 d . . .
N3 N 0.6802(2) -0.00845(9) 0.25118(9) 0.0159(3) Uani 1 1 d . . .
N2 N 0.3804(2) 0.17833(10) 0.23445(9) 0.0203(4) Uani 1 1 d . . .
N4 N 0.6771(2) -0.02794(10) 0.31704(9) 0.0176(4) Uani 1 1 d . . .
C17 C 0.6618(4) 0.07725(15) 0.47607(12) 0.0347(6) Uani 1 1 d . . .
H17A H 0.7740 0.0525 0.4853 0.052 Uiso 1 1 calc R . .
H17B H 0.5664 0.0428 0.4691 0.052 Uiso 1 1 calc R . .
H17C H 0.6496 0.1076 0.5149 0.052 Uiso 1 1 calc R . .
C3 C 0.2996(3) 0.23024(12) 0.19570(11) 0.0209(4) Uani 1 1 d . . .
C11 C 0.7434(3) -0.09319(11) 0.32480(11) 0.0174(4) Uani 1 1 d . . .
C18 C 0.7974(3) 0.16750(13) 0.42229(12) 0.0259(5) Uani 1 1 d . . .
H18A H 0.9091 0.1423 0.4365 0.031 Uiso 1 1 calc R . .
H18B H 0.7854 0.2036 0.4572 0.031 Uiso 1 1 calc R . .
C2 C 0.2328(3) 0.28036(11) 0.23485(11) 0.0212(4) Uani 1 1 d . . .
H2 H 0.1701 0.3220 0.2200 0.025 Uiso 1 1 calc R . .
C10 C 0.7912(3) -0.11794(11) 0.26489(11) 0.0179(4) Uani 1 1 d . . .
H10 H 0.8412 -0.1621 0.2567 0.021 Uiso 1 1 calc R . .
C19 C 0.7962(3) 0.20209(13) 0.35400(13) 0.0266(5) Uani 1 1 d . . .
H19A H 0.6943 0.2339 0.3432 0.032 Uiso 1 1 calc R . .
H19B H 0.9040 0.2301 0.3546 0.032 Uiso 1 1 calc R . .
C1 C 0.2790(3) 0.25530(11) 0.30105(11) 0.0166(4) Uani 1 1 d . . .
C9 C 0.7476(3) -0.06189(11) 0.21955(10) 0.0151(4) Uani 1 1 d . . .
C20 C 0.8307(4) 0.17095(15) 0.24076(13) 0.0326(6) Uani 1 1 d . . .
H20A H 0.7487 0.2078 0.2214 0.049 Uiso 1 1 calc R . .
H20B H 0.8242 0.1313 0.2088 0.049 Uiso 1 1 calc R . .
H20C H 0.9498 0.1900 0.2488 0.049 Uiso 1 1 calc R . .
C8 C 0.2807(4) 0.22723(14) 0.12037(13) 0.0328(6) Uani 1 1 d . . .
C16 C 0.7602(3) -0.12878(13) 0.39176(12) 0.0247(5) Uani 1 1 d . . .
C21 C 0.2288(3) 0.02825(14) 0.16036(12) 0.0290(5) Uani 1 1 d . . .
H21A H 0.2052 -0.0170 0.1369 0.044 Uiso 1 1 calc R . .
H21B H 0.3199 0.0534 0.1414 0.044 Uiso 1 1 calc R . .
H21C H 0.1217 0.0566 0.1539 0.044 Uiso 1 1 calc R . .
C4 C 0.2408(3) 0.28574(11) 0.36440(11) 0.0170(4) Uani 1 1 d . . .
C12 C 0.7733(3) -0.05645(11) 0.14875(10) 0.0163(4) Uani 1 1 d . . .
C22 C 0.1601(3) -0.02113(12) 0.26202(12) 0.0222(5) Uani 1 1 d . . .
H22A H 0.1273 -0.0655 0.2370 0.027 Uiso 1 1 calc R . .
H22B H 0.0535 0.0077 0.2612 0.027 Uiso 1 1 calc R . .
C5 C 0.1258(3) 0.34175(11) 0.37066(10) 0.0163(3) Uani 1 1 d . . .
H5 H 0.0635 0.3679 0.3336 0.020 Uiso 1 1 calc R . .
C13 C 0.8606(3) -0.10890(12) 0.11154(10) 0.0163(3) Uani 1 1 d . . .
H13 H 0.9074 -0.1530 0.1282 0.020 Uiso 1 1 calc R . .
C23 C 0.2435(3) -0.03658(12) 0.33459(12) 0.0214(4) Uani 1 1 d . . .
H23A H 0.1562 -0.0586 0.3591 0.026 Uiso 1 1 calc R . .
H23B H 0.3406 -0.0704 0.3346 0.026 Uiso 1 1 calc R . .
C6 C 0.1165(3) 0.35359(13) 0.44167(13) 0.0277(5) Uani 1 1 d . . .
H6 H 0.0443 0.3886 0.4568 0.033 Uiso 1 1 calc R . .
C14 C 0.8605(3) -0.07930(14) 0.04367(13) 0.0287(5) Uani 1 1 d . . .
H14 H 0.9128 -0.1030 0.0101 0.034 Uiso 1 1 calc R . .
C24 C 0.1740(3) 0.06755(13) 0.39185(13) 0.0281(5) Uani 1 1 d . . .
H24A H 0.0907 0.0832 0.3521 0.042 Uiso 1 1 calc R . .
H24B H 0.2259 0.1087 0.4173 0.042 Uiso 1 1 calc R . .
H24C H 0.1130 0.0388 0.4214 0.042 Uiso 1 1 calc R . .
C7 C 0.2203(4) 0.31017(13) 0.48484(13) 0.0307(5) Uani 1 1 d . . .
H7 H 0.2291 0.3116 0.5331 0.037 Uiso 1 1 calc R . .
C15 C 0.7813(3) -0.01604(14) 0.03175(12) 0.0295(5) Uani 1 1 d . . .
H15 H 0.7716 0.0082 -0.0105 0.035 Uiso 1 1 calc R . .
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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'
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
_geom_angle_publ_flag
N4 Ca1 O1 90.77(6) . . ?
N4 Ca1 O2 91.08(6) . . ?
O1 Ca1 O2 66.32(5) . . ?
N4 Ca1 N2 152.16(6) . . ?
O1 Ca1 N2 112.19(6) . . ?
O2 Ca1 N2 84.51(6) . . ?
N4 Ca1 O3 86.92(6) . . ?
O1 Ca1 O3 149.38(6) . . ?
O2 Ca1 O3 144.20(5) . . ?
N2 Ca1 O3 80.96(6) . . ?
N4 Ca1 N1 174.70(6) . . ?
O1 Ca1 N1 83.94(6) . . ?
O2 Ca1 N1 87.20(6) . . ?
N2 Ca1 N1 32.57(6) . . ?
O3 Ca1 N1 97.40(6) . . ?
N4 Ca1 N3 32.59(6) . . ?
O1 Ca1 N3 114.80(6) . . ?
O2 Ca1 N3 81.82(6) . . ?
N2 Ca1 N3 119.71(6) . . ?
O3 Ca1 N3 77.42(6) . . ?
N1 Ca1 N3 151.53(6) . . ?
N4 Ca1 O4 87.13(6) . . ?
O1 Ca1 O4 81.94(5) . . ?
O2 Ca1 O4 148.18(5) . . ?
N2 Ca1 O4 110.70(6) . . ?
O3 Ca1 O4 67.46(5) . . ?
N1 Ca1 O4 91.69(6) . . ?
N3 Ca1 O4 111.28(6) . . ?
N4 Ca1 C19 105.92(6) . . ?
O1 Ca1 C19 47.67(6) . . ?
O2 Ca1 C19 25.05(6) . . ?
N2 Ca1 C19 80.85(7) . . ?
O3 Ca1 C19 160.21(6) . . ?
N1 Ca1 C19 70.76(6) . . ?
N3 Ca1 C19 105.18(6) . . ?
O4 Ca1 C19 126.99(6) . . ?
N4 Ca1 C23 74.02(6) . . ?
O1 Ca1 C23 103.40(6) . . ?
O2 Ca1 C23 162.16(6) . . ?
N2 Ca1 C23 113.25(6) . . ?
O3 Ca1 C23 46.77(6) . . ?
N1 Ca1 C23 106.75(6) . . ?
N3 Ca1 C23 90.19(6) . . ?
O4 Ca1 C23 25.17(5) . . ?
C19 Ca1 C23 150.78(6) . . ?
C7 S1 C4 92.20(12) . . ?
C15 S2 C12 92.53(12) . . ?
C17 O1 C18 111.76(18) . . ?
C17 O1 Ca1 123.63(14) . . ?
C18 O1 Ca1 118.88(13) . . ?
C20 O2 C19 112.84(18) . . ?
C20 O2 Ca1 119.44(14) . . ?
C19 O2 Ca1 108.94(12) . . ?
C22 O3 C21 112.34(17) . . ?
C22 O3 Ca1 119.52(13) . . ?
C21 O3 Ca1 125.33(14) . . ?
C24 O4 C23 112.61(17) . . ?
C24 O4 Ca1 120.85(13) . . ?
C23 O4 Ca1 107.68(12) . . ?
C1 N1 N2 108.37(17) . . ?
C1 N1 Ca1 177.05(15) . . ?
N2 N1 Ca1 73.62(11) . . ?
C9 N3 N4 108.31(17) . . ?
C9 N3 Ca1 171.93(14) . . ?
N4 N3 Ca1 71.88(10) . . ?
C3 N2 N1 106.73(18) . . ?
C3 N2 Ca1 177.78(16) . . ?
N1 N2 Ca1 73.80(11) . . ?
C11 N4 N3 107.04(17) . . ?
C11 N4 Ca1 171.59(15) . . ?
N3 N4 Ca1 75.53(11) . . ?
N2 C3 C2 111.51(19) . . ?
N2 C3 C8 120.7(2) . . ?
C2 C3 C8 127.7(2) . . ?
N4 C11 C10 111.54(19) . . ?
N4 C11 C16 120.05(19) . . ?
C10 C11 C16 128.4(2) . . ?
O1 C18 C19 108.56(18) . . ?
C3 C2 C1 103.57(19) . . ?
C11 C10 C9 102.95(18) . . ?
O2 C19 C18 107.44(19) . . ?
O2 C19 Ca1 46.01(9) . . ?
C18 C19 Ca1 82.62(13) . . ?
N1 C1 C2 109.82(19) . . ?
N1 C1 C4 121.60(19) . . ?
C2 C1 C4 128.6(2) . . ?
N3 C9 C10 110.15(18) . . ?
N3 C9 C12 121.62(19) . . ?
C10 C9 C12 128.18(19) . . ?
F3 C8 F1 107.3(2) . . ?
F3 C8 F2 105.7(2) . . ?
F1 C8 F2 106.0(2) . . ?
F3 C8 C3 113.4(2) . . ?
F1 C8 C3 111.7(2) . . ?
F2 C8 C3 112.3(2) . . ?
F5 C16 F4 107.7(2) . . ?
F5 C16 F6 104.6(2) . . ?
F4 C16 F6 105.0(2) . . ?
F5 C16 C11 113.6(2) . . ?
F4 C16 C11 112.3(2) . . ?
F6 C16 C11 113.0(2) . . ?
C5 C4 C1 126.77(19) . . ?
C5 C4 S1 111.80(16) . . ?
C1 C4 S1 121.40(16) . . ?
C9 C12 C13 125.86(19) . . ?
C9 C12 S2 121.25(16) . . ?
C13 C12 S2 112.89(15) . . ?
O3 C22 C23 106.87(17) . . ?
C4 C5 C6 109.90(19) . . ?
C14 C13 C12 105.89(19) . . ?
O4 C23 C22 111.15(18) . . ?
O4 C23 Ca1 47.15(9) . . ?
C22 C23 Ca1 82.67(12) . . ?
C7 C6 C5 113.8(2) . . ?
C15 C14 C13 115.7(2) . . ?
C6 C7 S1 112.33(19) . . ?
C14 C15 S2 112.97(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 N4 2.4058(18) . ?
Ca1 O1 2.4272(15) . ?
Ca1 O2 2.4343(15) . ?
Ca1 N2 2.4352(19) . ?
Ca1 O3 2.4356(15) . ?
Ca1 N1 2.4374(18) . ?
Ca1 N3 2.4511(18) . ?
Ca1 O4 2.4746(15) . ?
Ca1 C19 3.200(2) . ?
Ca1 C23 3.216(2) . ?
S1 C7 1.705(3) . ?
S1 C4 1.720(2) . ?
S2 C15 1.690(3) . ?
S2 C12 1.712(2) . ?
F1 C8 1.336(3) . ?
F4 C16 1.321(3) . ?
F2 C8 1.342(3) . ?
F5 C16 1.318(3) . ?
F3 C8 1.333(3) . ?
F6 C16 1.338(3) . ?
O1 C17 1.422(3) . ?
O1 C18 1.427(3) . ?
O2 C20 1.429(3) . ?
O2 C19 1.433(3) . ?
O3 C22 1.424(3) . ?
O3 C21 1.425(3) . ?
O4 C24 1.434(3) . ?
O4 C23 1.436(3) . ?
N1 C1 1.351(3) . ?
N1 N2 1.366(3) . ?
N3 C9 1.345(3) . ?
N3 N4 1.364(2) . ?
N2 C3 1.341(3) . ?
N4 C11 1.341(3) . ?
C3 C2 1.384(3) . ?
C3 C8 1.480(3) . ?
C11 C10 1.387(3) . ?
C11 C16 1.478(3) . ?
C18 C19 1.506(4) . ?
C2 C1 1.388(3) . ?
C10 C9 1.399(3) . ?
C1 C4 1.460(3) . ?
C9 C12 1.457(3) . ?
C4 C5 1.408(3) . ?
C12 C13 1.472(3) . ?
C22 C23 1.507(3) . ?
C5 C6 1.442(3) . ?
C13 C14 1.461(3) . ?
C6 C7 1.354(4) . ?
C14 C15 1.353(4) . ?
