#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:12:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179317 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/14/4321449.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_4321449
loop_
_publ_author_name
'H. V. Rasika Dias'
'Sharon A. Polach'
_publ_section_title
;
 An Isolable, Oxygen-Coordinated Silver(I) Complex of Dimethyl
 Diazomalonate: Synthesis and Characterization of
 [HB(3,5-(CF3)2Pz)3]Ag[OC(OCH3)]2CN2 (Where Pz = Pyrazolyl)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4676
_journal_page_last               4677
_journal_paper_doi               10.1021/ic0002521
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C20 H10 Ag B F18 N8 O4'
_chemical_formula_weight         887.04
_chemical_name_common            '[HB(3,5-(CF3)2Pz)3]Ag(MeOCO)2CN2'
_chemical_name_systematic
; 

 ? 

;
_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                 102.550(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.9306(15)
_cell_length_b                   25.385(2)
_cell_length_c                   14.011(2)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      13.86
_cell_measurement_theta_min      4.99
_cell_volume                     3100.4(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_method       'ω 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  0.0220
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5233
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        4.23
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.802
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8438
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Rhomboid plates '
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         4045
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          1.561
_refine_ls_shift/su_mean         0.066
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0312P)²+2.6588P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                3209
_reflns_number_total             4045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0002521.cif
_cod_data_source_block           rd208
_cod_original_cell_volume        3100.6(8)
_cod_database_code               4321449
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
Ag Ag 0.10794(4) 0.192224(14) 0.26611(3) 0.05901(14) Uani 1 1 d . . .
N11 N 0.4214(3) 0.12794(12) 0.2522(2) 0.0386(8) Uani 1 1 d U . .
N12 N 0.3716(4) 0.17884(12) 0.2462(2) 0.0421(8) Uani 1 1 d U . .
N21 N 0.1772(4) 0.09075(13) 0.1453(2) 0.0411(8) Uani 1 1 d U . .
N22 N 0.0560(4) 0.12237(13) 0.1468(2) 0.0454(8) Uani 1 1 d U . .
N31 N 0.2360(4) 0.07656(12) 0.3300(2) 0.0402(8) Uani 1 1 d U . .
N32 N 0.1958(4) 0.11952(13) 0.3760(2) 0.0430(8) Uani 1 1 d U . .
C13 C 0.4968(5) 0.20844(16) 0.2659(3) 0.0449(10) Uani 1 1 d U A .
C14 C 0.6290(5) 0.17817(18) 0.2851(3) 0.0544(12) Uani 1 1 d U . .
H14A H 0.7302 0.1898 0.3009 0.065 Uiso 1 1 calc R . .
C15 C 0.5773(4) 0.12756(17) 0.2756(3) 0.0449(10) Uani 1 1 d U . .
C16 C 0.4825(6) 0.2664(2) 0.2638(4) 0.0682(15) Uani 1 1 d DU . .
C17 C 0.6705(5) 0.0787(2) 0.2895(4) 0.0634(13) Uani 1 1 d U . .
C23 C -0.0321(5) 0.12044(18) 0.0572(3) 0.0531(11) Uani 1 1 d U B .
C24 C 0.0298(5) 0.0887(2) -0.0033(3) 0.0632(13) Uani 1 1 d U . .
H24A H -0.0101 0.0814 -0.0690 0.076 Uiso 1 1 calc R . .
C25 C 0.1620(5) 0.07020(17) 0.0536(3) 0.0492(11) Uani 1 1 d U . .
C26 C -0.1810(6) 0.1495(2) 0.0344(4) 0.0756(15) Uani 1 1 d DU . .
C27 C 0.2750(7) 0.0346(2) 0.0243(4) 0.0716(15) Uani 1 1 d U . .
C33 C 0.1533(5) 0.10195(17) 0.4554(3) 0.0433(10) Uani 1 1 d U . .
C34 C 0.1647(6) 0.04814(18) 0.4627(3) 0.0601(13) Uani 1 1 d U . .
H34A H 0.1420 0.0268 0.5116 0.072 Uiso 1 1 calc R . .
C35 C 0.2168(5) 0.03295(17) 0.3823(3) 0.0549(12) Uani 1 1 d U . .
C36 C 0.1017(6) 0.1396(2) 0.5227(3) 0.0571(12) Uani 1 1 d U . .
C37 C 0.2492(9) -0.0216(2) 0.3538(5) 0.092(2) Uani 1 1 d U . .
F16A F 0.3745(15) 0.2846(3) 0.3102(8) 0.101(4) Uani 0.584(15) 1 d PDU A 1
F16B F 0.6025(10) 0.2929(4) 0.2955(13) 0.130(6) Uani 0.584(15) 1 d PDU A 1
F16C F 0.4211(13) 0.2841(4) 0.1738(5) 0.092(3) Uani 0.584(15) 1 d PDU A 1
F16D F 0.523(3) 0.2831(4) 0.3566(7) 0.138(7) Uani 0.416(15) 1 d PDU A 2
F16E F 0.6031(18) 0.2850(6) 0.2310(15) 0.117(6) Uani 0.416(15) 1 d PDU A 2
F16F F 0.3664(14) 0.2874(5) 0.222(2) 0.161(11) Uani 0.416(15) 1 d PDU A 2
F17A F 0.6438(4) 0.04914(14) 0.3621(2) 0.1004(11) Uani 1 1 d U . .
F17B F 0.8198(3) 0.09119(14) 0.3114(3) 0.1105(12) Uani 1 1 d U . .
F17C F 0.6513(3) 0.04808(12) 0.2127(2) 0.0851(9) Uani 1 1 d U . .
F26A F -0.2540(13) 0.1358(5) -0.0540(7) 0.112(5) Uani 0.542(15) 1 d PDU B 1
F26B F -0.2644(17) 0.1433(11) 0.0917(12) 0.217(11) Uani 0.542(15) 1 d PDU B 1
F26C F -0.1595(13) 0.1986(3) 0.0201(14) 0.143(8) Uani 0.542(15) 1 d PDU B 1
F26E F -0.1971(11) 0.1837(5) 0.1047(10) 0.099(5) Uani 0.458(15) 1 d PDU B 2
F26F F -0.208(2) 0.1766(10) -0.0405(13) 0.188(11) Uani 0.458(15) 1 d PDU B 2
F26D F -0.2958(12) 0.1180(4) 0.0357(18) 0.131(9) Uani 0.458(15) 1 d PDU B 2
F27A F 0.2318(4) 0.02294(17) -0.0700(2) 0.1213(14) Uani 1 1 d U . .
F27B F 0.2937(4) -0.01096(13) 0.0718(3) 0.0983(11) Uani 1 1 d U . .
F27C F 0.4137(4) 0.05602(14) 0.0368(2) 0.0927(10) Uani 1 1 d U . .
F36A F -0.0461(3) 0.15142(13) 0.4951(2) 0.0834(9) Uani 1 1 d U . .
F36B F 0.1222(4) 0.11976(13) 0.61207(19) 0.0974(11) Uani 1 1 d U . .
F36C F 0.1748(4) 0.18528(11) 0.5306(2) 0.0783(8) Uani 1 1 d U . .
F37A F 0.1863(6) -0.03238(13) 0.2627(3) 0.1358(18) Uani 1 1 d U . .
F37B F 0.3980(6) -0.03100(14) 0.3639(4) 0.1362(17) Uani 1 1 d U . .
F37C F 0.1968(5) -0.05602(12) 0.4102(3) 0.1286(15) Uani 1 1 d U . .
B B 0.3065(5) 0.08146(19) 0.2379(3) 0.0396(11) Uani 1 1 d . . .
H H 0.364(4) 0.0467(14) 0.226(2) 0.033(9) Uiso 1 1 d . . .
N1 N -0.0597(5) 0.38175(17) 0.2712(3) 0.0632(11) Uani 1 1 d U . .
N2 N -0.0836(8) 0.4243(2) 0.2770(4) 0.108(2) Uani 1 1 d U . .
O1 O -0.0293(4) 0.25054(12) 0.3503(2) 0.0563(8) Uani 1 1 d . . .
O2 O 0.0424(4) 0.26821(13) 0.1593(2) 0.0631(9) Uani 1 1 d . . .
O3 O -0.0995(4) 0.32593(11) 0.4125(2) 0.0558(8) Uani 1 1 d . . .
O4 O 0.0149(4) 0.35283(12) 0.1145(2) 0.0597(8) Uani 1 1 d . . .
C1 C -0.0322(5) 0.33032(16) 0.2639(3) 0.0448(10) Uani 1 1 d U . .
C2 C 0.0131(5) 0.31277(17) 0.1760(3) 0.0457(10) Uani 1 1 d U . .
C3 C -0.0511(5) 0.29758(17) 0.3452(3) 0.0438(10) Uani 1 1 d U . .
C4 C 0.0568(6) 0.3400(2) 0.0231(3) 0.0716(15) Uani 1 1 d U . .
H4A H 0.0380 0.3699 -0.0198 0.107 Uiso 1 1 calc R . .
H4B H -0.0034 0.3107 -0.0069 0.107 Uiso 1 1 calc R . .
H4C H 0.1637 0.3310 0.0354 0.107 Uiso 1 1 calc R . .
C5 C -0.1179(7) 0.2980(2) 0.4993(3) 0.0775(16) Uani 1 1 d U . .
H5A H -0.1631 0.3210 0.5396 0.116 Uiso 1 1 calc R . .
H5B H -0.0195 0.2863 0.5353 0.116 Uiso 1 1 calc R . .
H5C H -0.1834 0.2680 0.4807 0.116 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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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
O1 Ag N22 139.06(11) . . ?
O1 Ag N32 106.74(10) . . ?
N22 Ag N32 82.38(11) . . ?
O1 Ag O2 74.46(10) . . ?
N22 Ag O2 99.91(11) . . ?
N32 Ag O2 175.00(11) . . ?
O1 Ag N12 138.53(11) . . ?
N22 Ag N12 82.20(11) . . ?
N32 Ag N12 77.32(11) . . ?
O2 Ag N12 98.53(11) . . ?
C15 N11 N12 109.0(3) . . ?
C15 N11 B 129.9(3) . . ?
N12 N11 B 121.1(3) . . ?
C13 N12 N11 106.0(3) . . ?
C13 N12 Ag 133.2(3) . . ?
N11 N12 Ag 115.6(2) . . ?
N22 N21 C25 109.0(3) . . ?
N22 N21 B 121.9(3) . . ?
C25 N21 B 129.1(3) . . ?
C23 N22 N21 106.0(3) . . ?
C23 N22 Ag 131.8(3) . . ?
N21 N22 Ag 114.4(2) . . ?
N32 N31 C35 108.8(3) . . ?
N32 N31 B 121.7(3) . . ?
C35 N31 B 129.2(3) . . ?
C33 N32 N31 106.4(3) . . ?
C33 N32 Ag 132.6(3) . . ?
N31 N32 Ag 113.2(2) . . ?
N12 C13 C14 111.8(4) . . ?
N12 C13 C16 119.7(4) . . ?
C14 C13 C16 128.6(4) . . ?
C15 C14 C13 104.3(4) . . ?
N11 C15 C14 109.0(4) . . ?
N11 C15 C17 123.7(4) . . ?
C14 C15 C17 127.4(4) . . ?
F16F C16 F16B 120.8(9) . . ?
F16F C16 F16C 42.3(13) . . ?
F16B C16 F16C 107.1(8) . . ?
F16F C16 F16D 110.5(9) . . ?
F16B C16 F16D 57.4(7) . . ?
F16C C16 F16D 140.9(8) . . ?
F16F C16 F16E 110.5(10) . . ?
F16B C16 F16E 41.5(6) . . ?
F16C C16 F16E 75.8(9) . . ?
F16D C16 F16E 98.9(8) . . ?
F16F C16 F16A 56.6(12) . . ?
F16B C16 F16A 106.7(7) . . ?
F16C C16 F16A 98.6(6) . . ?
F16D C16 F16A 59.7(8) . . ?
F16E C16 F16A 138.5(8) . . ?
F16F C16 C13 121.1(7) . . ?
F16B C16 C13 117.4(7) . . ?
F16C C16 C13 111.7(6) . . ?
F16D C16 C13 107.0(6) . . ?
F16E C16 C13 106.5(7) . . ?
F16A C16 C13 113.5(5) . . ?
F17C C17 F17A 106.2(4) . . ?
F17C C17 F17B 106.0(4) . . ?
F17A C17 F17B 107.1(4) . . ?
F17C C17 C15 114.9(4) . . ?
F17A C17 C15 112.6(4) . . ?
F17B C17 C15 109.6(4) . . ?
N22 C23 C24 111.7(4) . . ?
N22 C23 C26 120.0(4) . . ?
C24 C23 C26 128.2(4) . . ?
C25 C24 C23 104.9(4) . . ?
C24 C25 N21 108.5(4) . . ?
C24 C25 C27 127.5(4) . . ?
N21 C25 C27 124.1(4) . . ?
F26B C26 F26F 126.8(9) . . ?
F26B C26 F26C 111.2(10) . . ?
F26F C26 F26C 48.3(10) . . ?
F26B C26 F26D 46.9(10) . . ?
F26F C26 F26D 110.2(9) . . ?
F26C C26 F26D 138.0(10) . . ?
F26B C26 F26A 109.8(10) . . ?
F26F C26 F26A 51.8(11) . . ?
F26C C26 F26A 99.9(7) . . ?
F26D C26 F26A 67.7(8) . . ?
F26B C26 F26E 54.6(11) . . ?
F26F C26 F26E 103.4(10) . . ?
F26C C26 F26E 62.0(7) . . ?
F26D C26 F26E 100.1(8) . . ?
F26A C26 F26E 138.7(7) . . ?
F26B C26 C23 116.0(7) . . ?
F26F C26 C23 117.2(7) . . ?
F26C C26 C23 110.9(7) . . ?
F26D C26 C23 111.1(8) . . ?
F26A C26 C23 107.9(6) . . ?
F26E C26 C23 113.2(6) . . ?
F27B C27 F27A 106.4(5) . . ?
F27B C27 F27C 106.2(5) . . ?
F27A C27 F27C 106.4(5) . . ?
F27B C27 C25 114.4(4) . . ?
F27A C27 C25 110.1(5) . . ?
F27C C27 C25 112.7(4) . . ?
N32 C33 C34 111.5(4) . . ?
N32 C33 C36 120.0(4) . . ?
C34 C33 C36 128.5(4) . . ?
C35 C34 C33 104.7(4) . . ?
N31 C35 C34 108.7(4) . . ?
N31 C35 C37 124.0(4) . . ?
C34 C35 C37 127.3(4) . . ?
F36C C36 F36B 106.8(4) . . ?
F36C C36 F36A 105.5(4) . . ?
F36B C36 F36A 106.6(4) . . ?
F36C C36 C33 113.7(4) . . ?
F36B C36 C33 110.9(4) . . ?
F36A C36 C33 112.7(4) . . ?
F37A C37 F37B 106.0(6) . . ?
F37A C37 F37C 108.2(6) . . ?
F37B C37 F37C 107.0(6) . . ?
F37A C37 C35 112.9(6) . . ?
F37B C37 C35 112.8(6) . . ?
F37C C37 C35 109.7(5) . . ?
N11 B N21 110.1(3) . . ?
N11 B N31 109.3(3) . . ?
N21 B N31 110.0(3) . . ?
N2 N1 C1 179.5(6) . . ?
C3 O1 Ag 132.5(3) . . ?
C2 O2 Ag 131.6(3) . . ?
C3 O3 C5 116.4(4) . . ?
C2 O4 C4 116.2(4) . . ?
N1 C1 C2 117.1(4) . . ?
N1 C1 C3 116.5(4) . . ?
C2 C1 C3 126.5(4) . . ?
O2 C2 O4 124.1(4) . . ?
O2 C2 C1 124.8(4) . . ?
O4 C2 C1 111.1(4) . . ?
O1 C3 O3 124.4(4) . . ?
O1 C3 C1 124.6(4) . . ?
O3 C3 C1 111.0(4) . . ?
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
Ag O1 2.390(3) . ?
Ag N22 2.412(3) . ?
Ag N32 2.422(3) . ?
Ag O2 2.434(3) . ?
Ag N12 2.454(3) . ?
N11 C15 1.359(5) . ?
N11 N12 1.363(4) . ?
N11 B 1.548(6) . ?
N12 C13 1.325(5) . ?
N21 N22 1.351(4) . ?
N21 C25 1.366(5) . ?
N21 B 1.556(6) . ?
N22 C23 1.330(5) . ?
N31 N32 1.354(4) . ?
N31 C35 1.359(5) . ?
N31 B 1.559(5) . ?
N32 C33 1.329(5) . ?
C13 C14 1.385(6) . ?
C13 C16 1.476(7) . ?
C14 C15 1.362(6) . ?
C15 C17 1.482(6) . ?
C16 F16F 1.198(9) . ?
C16 F16B 1.262(8) . ?
C16 F16C 1.339(9) . ?
C16 F16D 1.341(10) . ?
C16 F16E 1.345(10) . ?
C16 F16A 1.356(8) . ?
C17 F17C 1.308(5) . ?
C17 F17A 1.327(6) . ?
C17 F17B 1.339(6) . ?
C23 C24 1.369(6) . ?
C23 C26 1.494(7) . ?
C24 C25 1.357(6) . ?
C25 C27 1.478(7) . ?
C26 F26B 1.219(9) . ?
C26 F26F 1.233(9) . ?
C26 F26C 1.282(11) . ?
C26 F26D 1.304(10) . ?
C26 F26A 1.314(8) . ?
C26 F26E 1.344(9) . ?
C27 F27B 1.326(6) . ?
C27 F27A 1.328(5) . ?
C27 F27C 1.329(6) . ?
C33 C34 1.372(6) . ?
C33 C36 1.484(6) . ?
C34 C35 1.364(6) . ?
C35 C37 1.488(7) . ?
C36 F36C 1.323(5) . ?
C36 F36B 1.325(5) . ?
C36 F36A 1.327(5) . ?
C37 F37A 1.306(8) . ?
C37 F37B 1.327(8) . ?
C37 F37C 1.329(6) . ?
N1 N2 1.108(6) . ?
N1 C1 1.336(6) . ?
O1 C3 1.210(5) . ?
O2 C2 1.195(5) . ?
O3 C3 1.330(5) . ?
O3 C5 1.449(5) . ?
O4 C2 1.335(5) . ?
O4 C4 1.447(5) . ?
C1 C2 1.448(6) . ?
C1 C3 1.449(6) . ?
