#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:27:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179329 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/26/4322662.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_4322662
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           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   14.461(2)
_cell_length_b                   14.461(2)
_cell_length_c                   30.473(3)
_cell_measurement_temperature    293(2)
_cell_volume                     5518.8(12)
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4682
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    0.615
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_F_000             1920
_refine_diff_density_max         1.206
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.316
_refine_ls_goodness_of_fit_obs   1.396
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.430
_refine_ls_restrained_S_obs      1.396
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_obs          0.0553
_refine_ls_shift/esd_max         0.017
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2015
_refine_ls_wR_factor_obs         0.1761
_reflns_number_observed          2377
_reflns_number_total             2957
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9707624_2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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_sg_symbol_H-M      'R -3'
_cod_database_code               4322662
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 0.6667 0.3333 0.146244(12) 0.0501(2) Uani 1 d S .
P1 P 0.6667 0.3333 0.22397(4) 0.0360(3) Uani 1 d S .
N1 N 0.5823(3) 0.3902(3) 0.09558(10) 0.0593(8) Uani 1 d . .
N2 N 0.5887(3) 0.3690(3) 0.05304(10) 0.0618(8) Uani 1 d . .
C1 C 0.5195(4) 0.3852(4) 0.0292(2) 0.0768(13) Uani 1 d . .
C2 C 0.4675(4) 0.4174(4) 0.0561(2) 0.0806(14) Uani 1 d . .
C3 C 0.5086(4) 0.4201(4) 0.0975(2) 0.0669(11) Uani 1 d . .
C4 C 0.5411(2) 0.3093(2) 0.24849(9) 0.0389(6) Uani 1 d . .
C5 C 0.5419(3) 0.3765(3) 0.28212(11) 0.0481(7) Uani 1 d . .
C6 C 0.4472(3) 0.3596(4) 0.29982(13) 0.0615(10) Uani 1 d . .
C7 C 0.3518(3) 0.2793(4) 0.28545(15) 0.0677(11) Uani 1 d . .
C8 C 0.3490(3) 0.2114(4) 0.25297(13) 0.0595(9) Uani 1 d . .
C9 C 0.4432(3) 0.2253(3) 0.23359(11) 0.0488(7) Uani 1 d . .
C10 C 0.4356(3) 0.1464(4) 0.1999(2) 0.0687(12) Uani 1 d . .
B1 B 0.6667 0.3333 0.0367(3) 0.068(2) Uani 1 d S .
H1 H 0.5153 0.3700 -0.0053 0.096(18) Uiso 1 d . .
H2 H 0.4063 0.4377 0.0515 0.085(15) Uiso 1 d . .
H3 H 0.4842 0.4208 0.1230 0.073(15) Uiso 1 d . .
H1B H 0.6667 0.3333 0.0040 0.063(20) Uiso 1 d S .
H5 H 0.6048 0.3599 0.3337 0.093(17) Uiso 1 d . .
H6 H 0.4495 0.3987 0.3156 0.056(12) Uiso 1 d . .
H7 H 0.2852 0.2779 0.3000 0.074(13) Uiso 1 d . .
H8 H 0.2738 0.1420 0.2521 0.077(15) Uiso 1 d . .
H10A H 0.5261 0.0567 0.2193 0.188(40) Uiso 1 d . .
H10B H 0.4274 0.1872 0.1748 0.127(25) Uiso 1 d . .
H10C H 0.3479 0.0729 0.2172 0.147(26) 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
N1 Ag N1 81.72(13) 2_655 3_665 ?
N1 Ag N1 81.71(13) 2_655 . ?
N1 Ag N1 81.70(13) 3_665 . ?
N1 Ag P1 130.95(8) 2_655 . ?
N1 Ag P1 130.95(8) 3_665 . ?
N1 Ag P1 130.93(8) . . ?
C4 P1 C4 104.48(11) 2_655 3_665 ?
C4 P1 C4 104.46(11) 2_655 . ?
C4 P1 C4 104.42(11) 3_665 . ?
C4 P1 Ag 114.13(10) 2_655 . ?
C4 P1 Ag 114.12(10) 3_665 . ?
C4 P1 Ag 114.11(10) . . ?
C3 N1 N2 105.8(3) . . ?
C3 N1 Ag 136.1(3) . . ?
N2 N1 Ag 116.5(3) . . ?
N1 N2 C1 109.8(4) . . ?
N1 N2 B1 122.2(4) . . ?
C1 N2 B1 128.0(5) . . ?
C2 C1 N2 108.8(4) . . ?
C1 C2 C3 105.1(4) . . ?
N1 C3 C2 110.5(4) . . ?
C9 C4 C5 119.3(3) . . ?
C9 C4 P1 120.6(2) . . ?
C5 C4 P1 120.1(2) . . ?
C6 C5 C4 119.9(3) . . ?
C7 C6 C5 121.4(4) . . ?
C6 C7 C8 119.8(4) . . ?
C7 C8 C9 121.2(4) . . ?
C4 C9 C8 118.3(3) . . ?
C4 C9 C10 122.7(3) . . ?
C8 C9 C10 118.9(3) . . ?
N2 B1 N2 110.1(3) 2_655 3_665 ?
N2 B1 N2 110.1(3) 2_655 . ?
N2 B1 N2 110.0(3) 3_665 . ?
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 N1 2.355(3) 2_655 ?
Ag N1 2.356(3) 3_665 ?
Ag N1 2.356(3) . ?
Ag P1 2.3685(13) . ?
P1 C4 1.828(3) 2_655 ?
P1 C4 1.829(3) 3_665 ?
P1 C4 1.829(3) . ?
N1 C3 1.338(6) . ?
N1 N2 1.346(4) . ?
N2 C1 1.349(6) . ?
N2 B1 1.539(5) . ?
C1 C2 1.344(8) . ?
C2 C3 1.386(7) . ?
C4 C9 1.402(5) . ?
C4 C5 1.408(5) . ?
C5 C6 1.376(5) . ?
C6 C7 1.357(6) . ?
C7 C8 1.379(6) . ?
C8 C9 1.405(5) . ?
C9 C10 1.497(5) . ?
B1 N2 1.539(5) 2_655 ?
B1 N2 1.539(5) 3_665 ?
