#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:18:17 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179659 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/12/4511270.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_4511270
loop_
_publ_author_name
'Durá, Gema'
'Carrión, M. Carmen'
'Jalón, Félix A.'
'Rodríguez, Ana M.'
'Manzano, Blanca R.'
_publ_section_title
;
 Metal Supramolecular Frameworks with Silver and Ditopic
 Bis(pyrazolyl)methane Ligands: Effect of the Anions and Ligand
 Substitution
;
_journal_issue                   7
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3510
_journal_paper_doi               10.1021/cg5004484
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C32 H38 Ag2 F4 N10 O4 P2'
_chemical_formula_weight         980.40
_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
_audit_creation_method           SHELXL--97
_cell_angle_alpha                90
_cell_angle_beta                 104.689(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.674(7)
_cell_length_b                   24.68(2)
_cell_length_c                   9.388(8)
_cell_measurement_reflns_used    618
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      15.040
_cell_measurement_theta_min      2.389
_cell_volume                     1944(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2259
_diffrn_reflns_av_sigmaI/netI    0.2289
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12373
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.159
_exptl_absorpt_correction_T_max  0.934
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.872
_refine_ls_R_factor_all          0.2368
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1195P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.2595
_reflns_number_gt                1202
_reflns_number_total             3385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5004484_si_002.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 4511266--4511274.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4511270
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 1.02255(14) 0.39711(4) 0.21753(15) 0.0744(6) Uani 1 1 d . . . . .
P1 P 1.2835(6) 0.3934(2) 0.5591(6) 0.0865(14) Uani 1 1 d . . . . .
N1 N 0.7516(15) 0.3900(5) 0.2035(15) 0.067(3) Uani 1 1 d . . . . .
N2 N 0.6558(13) 0.3720(4) 0.0720(15) 0.054(3) Uani 1 1 d . . . . .
N3 N 0.9580(13) 0.3208(4) 0.0705(12) 0.056(3) Uani 1 1 d . . . . .
N4 N 0.8225(14) 0.3228(4) -0.0453(12) 0.050(3) Uani 1 1 d . . . . .
N5 N 1.1238(15) 0.4786(4) 0.1780(14) 0.065(3) Uani 1 1 d . . . . .
C1 C 0.5104(17) 0.3567(5) 0.093(2) 0.064(4) Uani 1 1 d . . . . .
C2 C 0.515(2) 0.3680(6) 0.232(2) 0.080(5) Uani 1 1 d . . . . .
H2 H 0.4330 0.3628 0.2775 0.096 Uiso 1 1 calc R U . . .
C3 C 0.666(2) 0.3891(6) 0.2978(19) 0.068(4) Uani 1 1 d . . . . .
C4 C 0.3831(18) 0.3358(6) -0.0253(19) 0.086(5) Uani 1 1 d . . . . .
H4A H 0.4201 0.3323 -0.1130 0.130 Uiso 1 1 calc R U . . .
H4B H 0.2942 0.3603 -0.0433 0.130 Uiso 1 1 calc R U . . .
H4C H 0.3507 0.3010 0.0022 0.130 Uiso 1 1 calc R U . . .
C5 C 0.738(2) 0.4039(8) 0.453(2) 0.122(7) Uani 1 1 d . . . . .
H5A H 0.8444 0.4172 0.4624 0.182 Uiso 1 1 calc R U . . .
H5B H 0.7422 0.3725 0.5142 0.182 Uiso 1 1 calc R U . . .
H5C H 0.6751 0.4315 0.4827 0.182 Uiso 1 1 calc R U . . .
C6 C 0.8043(18) 0.2780(5) -0.1266(19) 0.065(4) Uani 1 1 d . . . . .
C7 C 0.9261(19) 0.2449(6) -0.0661(19) 0.074(5) Uani 1 1 d . . . . .
H7 H 0.9449 0.2107 -0.0994 0.089 Uiso 1 1 calc R U . . .
C8 C 1.0190(18) 0.2719(5) 0.0560(17) 0.058(4) Uani 1 1 d . . . . .
C9 C 0.674(2) 0.2686(6) -0.263(2) 0.095(6) Uani 1 1 d . . . . .
H9A H 0.6041 0.2995 -0.2807 0.143 Uiso 1 1 calc R U . . .
H9B H 0.6142 0.2370 -0.2497 0.143 Uiso 1 1 calc R U . . .
H9C H 0.7189 0.2633 -0.3450 0.143 Uiso 1 1 calc R U . . .
C10 C 1.1614(18) 0.2551(6) 0.1724(17) 0.082(5) Uani 1 1 d . . . . .
H10A H 1.1958 0.2847 0.2394 0.123 Uiso 1 1 calc R U . . .
H10B H 1.2456 0.2453 0.1279 0.123 Uiso 1 1 calc R U . . .
H10C H 1.1349 0.2246 0.2250 0.123 Uiso 1 1 calc R U . . .
C11 C 0.7118(16) 0.3664(5) -0.0579(17) 0.056(4) Uani 1 1 d . . . . .
H11 H 0.6194 0.3575 -0.1390 0.067 Uiso 1 1 calc R U . . .
C12 C 0.7770(17) 0.4216(5) -0.0949(15) 0.054(4) Uani 1 1 d . . . . .
C13 C 0.7056(18) 0.4679(5) -0.0743(19) 0.079(5) Uani 1 1 d . . . . .
H13 H 0.6195 0.4674 -0.0322 0.095 Uiso 1 1 calc R U . . .
C14 C 0.760(2) 0.5167(6) -0.116(2) 0.087(6) Uani 1 1 d . . . . .
H14 H 0.7097 0.5482 -0.0973 0.104 Uiso 1 1 calc R U . . .
C15 C 0.9433(17) 0.4758(6) -0.1996(16) 0.069(4) Uani 1 1 d . . . . .
H15 H 1.0276 0.4775 -0.2440 0.083 Uiso 1 1 calc R U . . .
C16 C 0.8978(18) 0.4251(5) -0.1609(18) 0.066(4) Uani 1 1 d . . . . .
H16 H 0.9499 0.3941 -0.1801 0.079 Uiso 1 1 calc R U . . .
O1 O 1.2079(14) 0.3662(5) 0.4241(13) 0.097(4) Uani 1 1 d . . . . .
O2 O 1.4325(13) 0.3762(5) 0.6564(13) 0.096(4) Uani 1 1 d . . . . .
F1 F 1.1484(19) 0.3809(8) 0.651(2) 0.081(6) Uani 0.5 1 d . . P A 1
F2 F 1.240(3) 0.4543(7) 0.553(3) 0.133(9) Uani 0.5 1 d . . P A 1
F2A F 1.344(3) 0.4498(10) 0.500(3) 0.123(9) Uiso 0.5 1 d . . P A 2
F1A F 1.204(5) 0.418(2) 0.651(5) 0.220(19) Uiso 0.5 1 d . . P A 2
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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
N5 Ag1 N3 132.1(4) . .
N5 Ag1 O1 102.4(4) . .
N3 Ag1 O1 104.0(4) . .
N5 Ag1 N1 119.1(4) . .
N3 Ag1 N1 79.4(4) . .
O1 Ag1 N1 120.0(4) . .
F1A P1 O1 125(2) . .
F1A P1 O2 104(2) . .
O1 P1 O2 123.7(8) . .
O1 P1 F2 111.5(12) . .
O2 P1 F2 118.9(11) . .
F1A P1 F2A 95(2) . .
O1 P1 F2A 102.3(10) . .
O2 P1 F2A 98.7(11) . .
O1 P1 F1 98.6(9) . .
O2 P1 F1 104.7(8) . .
F2 P1 F1 90.1(12) . .
C3 N1 N2 106.8(12) . .
C3 N1 Ag1 135.2(11) . .
N2 N1 Ag1 116.5(9) . .
N1 N2 C1 109.2(12) . .
N1 N2 C11 122.6(11) . .
C1 N2 C11 128.0(14) . .
C8 N3 N4 103.4(11) . .
C8 N3 Ag1 138.7(10) . .
N4 N3 Ag1 117.8(7) . .
C6 N4 N3 111.9(11) . .
C6 N4 C11 126.9(13) . .
N3 N4 C11 120.8(11) . .
C15 N5 C14 115.0(13) 3_765 3_765
C15 N5 Ag1 122.2(10) 3_765 .
C14 N5 Ag1 122.2(11) 3_765 .
C2 C1 N2 106.2(15) . .
C2 C1 C4 131.1(16) . .
N2 C1 C4 122.6(17) . .
C1 C2 C3 107.9(17) . .
N1 C3 C2 109.8(15) . .
N1 C3 C5 119.9(15) . .
C2 C3 C5 130.0(18) . .
N4 C6 C7 107.3(15) . .
N4 C6 C9 125.0(13) . .
C7 C6 C9 127.7(14) . .
C6 C7 C8 106.7(13) . .
N3 C8 C7 110.7(13) . .
N3 C8 C10 116.9(13) . .
C7 C8 C10 132.3(13) . .
N2 C11 N4 111.7(11) . .
N2 C11 C12 109.1(11) . .
N4 C11 C12 114.0(10) . .
C16 C12 C13 117.0(13) . .
C16 C12 C11 122.0(13) . .
C13 C12 C11 120.8(13) . .
C12 C13 C14 120.0(14) . .
N5 C14 C13 124.4(14) 3_765 .
N5 C15 C16 124.6(13) 3_765 .
C12 C16 C15 118.9(14) . .
P1 O1 Ag1 130.6(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N5 2.264(11) .
Ag1 N3 2.319(11) .
Ag1 O1 2.312(12) .
Ag1 N1 2.327(13) .
P1 F1A 1.38(5) .
P1 O1 1.437(12) .
P1 O2 1.444(12) .
P1 F2 1.548(17) .
P1 F2A 1.64(2) .
P1 F1 1.652(18) .
N1 C3 1.290(17) .
N1 N2 1.375(15) .
N2 C1 1.377(17) .
N2 C11 1.430(16) .
N3 C8 1.339(15) .
N3 N4 1.385(14) .
N4 C6 1.330(16) .
N4 C11 1.426(15) .
N5 C15 1.305(16) 3_765
N5 C14 1.292(18) 3_765
C1 C2 1.33(2) .
C1 C4 1.45(2) .
C2 C3 1.40(2) .
C3 C5 1.48(2) .
C6 C7 1.342(19) .
C6 C9 1.50(2) .
C7 C8 1.39(2) .
C8 C10 1.486(19) .
C11 C12 1.550(18) .
C12 C16 1.349(18) .
C12 C13 1.337(17) .
C13 C14 1.384(19) .
C14 N5 1.292(18) 3_765
C15 N5 1.305(16) 3_765
C15 C16 1.388(18) .
