#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:27:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179329 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322663.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_4322663
loop_
_publ_author_name
'C. Santini'
'G. Gioia Lobbia'
'C. Pettinari'
'M. Pellei'
'G. Valle'
'S. Calogero'
_publ_section_title
;
 Syntheses and Spectroscopic and Structural Characterization of Silver(I)
 Complexes Containing Tertiary Phosphines and Hydrotris(pyrazol-1-yl)-,
 Hydrotris(4-bromopyrazol-1-yl)-, Hydrotris(3,5-dimethypyrazol-1-yl)-, and
 Hydrotris(3-methyl-2-thioxo-1-imidazolyl)borates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              890
_journal_page_last               900
_journal_paper_doi               10.1021/ic9707624
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C30 H31 Ag B N6 P'
_chemical_formula_weight         625.26
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.80(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.183(2)
_cell_length_b                   18.596(2)
_cell_length_c                   13.804(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3072.0(13)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7488
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.737
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_F_000             1280
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.811
_refine_ls_goodness_of_fit_obs   0.986
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.811
_refine_ls_restrained_S_obs      0.986
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_obs          0.0408
_refine_ls_shift/esd_max         0.110
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0587P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1201
_refine_ls_wR_factor_obs         0.0908
_reflns_number_observed          3034
_reflns_number_total             7188
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9707624_3.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3072.0(7)
_cod_database_code               4322663
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ag Ag 0.72255(3) 0.28582(2) 0.56669(3) 0.06334(14) Uani 1 d . .
P P 0.58462(9) 0.20546(6) 0.49485(8) 0.0533(3) Uani 1 d . .
N1 N 0.7476(3) 0.3957(2) 0.4911(3) 0.0620(10) Uani 1 d . .
N2 N 0.8318(3) 0.4389(2) 0.5365(3) 0.0589(9) Uani 1 d . .
N3 N 0.9213(3) 0.2842(2) 0.5915(3) 0.0670(10) Uani 1 d . .
N4 N 0.9730(3) 0.3471(2) 0.6197(3) 0.0589(9) Uani 1 d . .
N5 N 0.7612(3) 0.3537(2) 0.7132(3) 0.0641(10) Uani 1 d . .
N6 N 0.8389(3) 0.4065(2) 0.7162(2) 0.0583(9) Uani 1 d . .
C1 C 0.8349(4) 0.4985(3) 0.4846(4) 0.0657(13) Uani 1 d . .
C2 C 0.7513(4) 0.4946(3) 0.4022(4) 0.0750(15) Uani 1 d . .
C3 C 0.7015(4) 0.4301(3) 0.4109(4) 0.0618(12) Uani 1 d . .
C4 C 1.0025(5) 0.2378(4) 0.5837(4) 0.080(2) Uani 1 d . .
C5 C 1.1063(5) 0.2697(4) 0.6069(4) 0.086(2) Uani 1 d . .
C6 C 1.0854(4) 0.3384(4) 0.6290(4) 0.0728(15) Uani 1 d . .
C7 C 0.7163(4) 0.3628(3) 0.7937(4) 0.0695(13) Uani 1 d . .
C8 C 0.7639(5) 0.4204(3) 0.8470(4) 0.078(2) Uani 1 d . .
C9 C 0.8392(5) 0.4464(3) 0.7964(4) 0.0689(13) Uani 1 d . .
C10 C 0.5643(5) 0.1220(3) 0.5610(4) 0.0688(14) Uani 1 d . .
C11 C 0.5287(3) 0.1346(2) 0.6581(2) 0.0574(11) Uani 1 d G .
C12 C 0.6072(2) 0.1532(2) 0.7409(3) 0.0755(14) Uani 1 d G .
C13 C 0.5741(4) 0.1638(2) 0.8309(2) 0.092(2) Uani 1 d G .
C14 C 0.4624(4) 0.1558(2) 0.8380(2) 0.099(2) Uani 1 d G .
C15 C 0.3839(3) 0.1372(2) 0.7552(3) 0.103(2) Uani 1 d G .
C16 C 0.4171(2) 0.1266(2) 0.6652(3) 0.0805(15) Uani 1 d G .
C17 C 0.4401(4) 0.2410(3) 0.4651(4) 0.0701(14) Uani 1 d . .
C18 C 0.4280(3) 0.3124(2) 0.4136(3) 0.0636(12) Uani 1 d G .
C19 C 0.4200(3) 0.3151(2) 0.3119(3) 0.0769(14) Uani 1 d G .
C20 C 0.4054(3) 0.3807(3) 0.2630(3) 0.094(2) Uani 1 d G .
C21 C 0.3988(3) 0.4437(2) 0.3159(4) 0.101(2) Uani 1 d G .
C22 C 0.4069(3) 0.4411(2) 0.4176(4) 0.098(2) Uani 1 d G .
C23 C 0.4215(3) 0.3754(2) 0.4665(3) 0.082(2) Uani 1 d G .
C24 C 0.6037(4) 0.1703(3) 0.3743(4) 0.0658(13) Uani 1 d . .
C25 C 0.7116(3) 0.1319(2) 0.3759(3) 0.0648(12) Uani 1 d G .
C26 C 0.8053(4) 0.1711(2) 0.3639(3) 0.100(2) Uani 1 d G .
C27 C 0.9057(3) 0.1361(4) 0.3623(4) 0.139(3) Uani 1 d G .
C28 C 0.9125(4) 0.0618(4) 0.3728(4) 0.134(3) Uani 1 d G .
C29 C 0.8189(5) 0.0225(2) 0.3848(4) 0.122(2) Uani 1 d G .
C30 C 0.7184(4) 0.0576(2) 0.3863(3) 0.096(2) Uani 1 d G .
B1 B 0.9091(4) 0.4165(3) 0.6340(4) 0.0614(14) Uani 1 d . .
H1B1 H 0.9636(28) 0.4552(18) 0.6547(23) 0.044(10) Uiso 1 d . .
H1 H 0.8849(37) 0.5344(24) 0.5047(32) 0.079(15) Uiso 1 d . .
H2 H 0.7389(45) 0.5281(29) 0.3601(40) 0.111(22) Uiso 1 d . .
H3 H 0.6423(31) 0.4113(19) 0.3711(27) 0.046(11) Uiso 1 d . .
H4 H 0.9864(32) 0.1914(22) 0.5718(28) 0.048(13) Uiso 1 d . .
H5 H 1.1745(42) 0.2529(27) 0.6023(35) 0.089(17) Uiso 1 d . .
H6 H 1.1269(38) 0.3794(24) 0.6507(33) 0.077(16) Uiso 1 d . .
H7 H 0.6638(35) 0.3322(22) 0.7998(30) 0.062(14) Uiso 1 d . .
H8 H 0.7528(36) 0.4383(26) 0.9067(35) 0.087(16) Uiso 1 d . .
H9 H 0.8835(36) 0.4862(24) 0.8051(32) 0.073(15) Uiso 1 d . .
H10A H 0.6343(36) 0.1011(21) 0.5758(30) 0.062(14) Uiso 1 d . .
H10B H 0.5199(36) 0.0908(22) 0.5241(31) 0.065(14) Uiso 1 d . .
H12 H 0.6884(52) 0.1642(34) 0.7307(46) 0.159(25) Uiso 1 d . .
H13 H 0.6245(52) 0.1789(34) 0.8845(45) 0.140(23) Uiso 1 d . .
H14 H 0.4534(46) 0.1635(30) 0.9047(42) 0.127(21) Uiso 1 d . .
H15 H 0.3826(134) 0.1476(95) 0.7869(132) 0.440(92) Uiso 1 d . .
H16 H 0.3616(46) 0.1141(29) 0.5955(41) 0.135(22) Uiso 1 d . .
H17A H 0.4264(30) 0.2433(21) 0.5265(29) 0.053(12) Uiso 1 d . .
H17B H 0.3941(34) 0.2030(21) 0.4248(31) 0.066(13) Uiso 1 d . .
H19 H 0.4186(36) 0.2706(23) 0.2692(33) 0.083(16) Uiso 1 d . .
H20 H 0.3993(44) 0.3874(28) 0.1858(41) 0.124(20) Uiso 1 d . .
H21 H 0.3972(40) 0.4915(27) 0.2819(36) 0.105(18) Uiso 1 d . .
H22 H 0.3899(43) 0.4856(28) 0.4426(39) 0.116(20) Uiso 1 d . .
H23 H 0.4332(41) 0.3721(26) 0.5351(37) 0.104(18) Uiso 1 d . .
H24A H 0.5955(35) 0.2116(22) 0.3360(32) 0.067(14) Uiso 1 d . .
H24B H 0.5423(35) 0.1374(22) 0.3543(29) 0.066(13) Uiso 1 d . .
H26 H 0.7939(43) 0.2353(29) 0.3492(39) 0.127(21) Uiso 1 d . .
H27 H 0.9776(104) 0.1516(63) 0.3749(94) 0.333(61) Uiso 1 d . .
H28 H 0.9673(54) 0.0390(39) 0.3842(55) 0.164(30) Uiso 1 d . .
H29 H 0.8309(60) -0.0330(38) 0.3867(52) 0.182(31) Uiso 1 d . .
H30 H 0.6742(100) 0.0458(62) 0.3833(92) 0.316(58) Uiso 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ag Ag -0.8971 1.1015 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
P Ag N1 120.99(10) . . ?
P Ag N5 136.23(11) . . ?
N1 Ag N5 83.86(12) . . ?
P Ag N3 133.36(11) . . ?
N1 Ag N3 82.01(13) . . ?
N5 Ag N3 81.3(2) . . ?
C24 P C10 101.5(3) . . ?
C24 P C17 101.6(3) . . ?
C10 P C17 101.5(3) . . ?
C24 P Ag 114.2(2) . . ?
C10 P Ag 118.9(2) . . ?
C17 P Ag 116.5(2) . . ?
C3 N1 N2 105.5(4) . . ?
C3 N1 Ag 137.0(3) . . ?
N2 N1 Ag 117.5(3) . . ?
C1 N2 N1 109.9(4) . . ?
C1 N2 B1 128.5(4) . . ?
N1 N2 B1 121.6(4) . . ?
C4 N3 N4 105.7(4) . . ?
C4 N3 Ag 138.3(4) . . ?
N4 N3 Ag 115.9(3) . . ?
N3 N4 C6 109.2(4) . . ?
N3 N4 B1 122.9(3) . . ?
C6 N4 B1 127.8(5) . . ?
C7 N5 N6 105.9(4) . . ?
C7 N5 Ag 137.2(3) . . ?
N6 N5 Ag 116.1(3) . . ?
C9 N6 N5 108.8(4) . . ?
C9 N6 B1 128.5(4) . . ?
N5 N6 B1 122.7(4) . . ?
N2 C1 C2 108.1(5) . . ?
C3 C2 C1 104.2(5) . . ?
N1 C3 C2 112.2(5) . . ?
N3 C4 C5 111.4(6) . . ?
C6 C5 C4 104.9(5) . . ?
C5 C6 N4 108.7(5) . . ?
N5 C7 C8 110.4(5) . . ?
C9 C8 C7 105.4(5) . . ?
N6 C9 C8 109.5(5) . . ?
C11 C10 P 113.5(3) . . ?
C12 C11 C16 120.0 . . ?
C12 C11 C10 120.3(3) . . ?
C16 C11 C10 119.7(3) . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C14 120.0 . . ?
C13 C14 C15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C11 120.0 . . ?
C18 C17 P 115.2(3) . . ?
C19 C18 C23 120.0 . . ?
C19 C18 C17 119.5(3) . . ?
C23 C18 C17 120.5(3) . . ?
C20 C19 C18 120.0 . . ?
C19 C20 C21 120.0 . . ?
C20 C21 C22 120.0 . . ?
C23 C22 C21 120.0 . . ?
C22 C23 C18 120.0 . . ?
C25 C24 P 114.6(3) . . ?
C26 C25 C30 120.0 . . ?
C26 C25 C24 119.2(4) . . ?
C30 C25 C24 120.8(4) . . ?
C25 C26 C27 120.0 . . ?
C28 C27 C26 120.0 . . ?
C29 C28 C27 120.0 . . ?
C30 C29 C28 120.0 . . ?
C29 C30 C25 120.0 . . ?
N4 B1 N2 110.8(4) . . ?
N4 B1 N6 110.7(4) . . ?
N2 B1 N6 109.8(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 P 2.327(2) . ?
Ag N1 2.340(4) . ?
Ag N5 2.356(4) . ?
Ag N3 2.382(4) . ?
P C24 1.842(5) . ?
P C10 1.841(5) . ?
P C17 1.853(5) . ?
N1 C3 1.310(5) . ?
N1 N2 1.360(4) . ?
N2 C1 1.323(5) . ?
N2 B1 1.549(6) . ?
N3 C4 1.333(6) . ?
N3 N4 1.352(4) . ?
N4 C6 1.361(6) . ?
N4 B1 1.538(6) . ?
N5 C7 1.337(6) . ?
N5 N6 1.359(4) . ?
N6 C9 1.332(6) . ?
N6 B1 1.555(6) . ?
C1 C2 1.379(7) . ?
C2 C3 1.360(7) . ?
C4 C5 1.379(8) . ?
C5 C6 1.348(8) . ?
C7 C8 1.366(7) . ?
C8 C9 1.344(7) . ?
C10 C11 1.502(6) . ?
C11 C12 1.39 . ?
C11 C16 1.39 . ?
C12 C13 1.39 . ?
C13 C14 1.39 . ?
C14 C15 1.39 . ?
C15 C16 1.39 . ?
C17 C18 1.500(6) . ?
C18 C19 1.39 . ?
C18 C23 1.39 . ?
C19 C20 1.39 . ?
C20 C21 1.39 . ?
C21 C22 1.39 . ?
C22 C23 1.39 . ?
C24 C25 1.494(6) . ?
C25 C26 1.39 . ?
C25 C30 1.39 . ?
C26 C27 1.39 . ?
C27 C28 1.39 . ?
C28 C29 1.39 . ?
C29 C30 1.39 . ?
