#------------------------------------------------------------------------------
#$Date: 2017-02-14 09:47:09 +0200 (Tue, 14 Feb 2017) $
#$Revision: 192057 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/01/4300100.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_4300100
loop_
_publ_author_name
'Susan Lorenzo'
'Caitlin Horn'
'Donald Craig'
'Marcia Scudder'
'Ian Dance'
_publ_section_title
;
Crystal Supramolecular Motifs: Columns of Embracing Ph3PMe+ or
Ph3PCl+ Cations Controlling Formation of [Cu3X82- (X = Cl, Br)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              401
_journal_page_last               405
_journal_paper_doi               10.1021/ic990803r
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         '2(C19 H18 P +1), Cu3 Br8 2-'
_chemical_formula_sum            'C38 H36 Br8 Cu3 P2'
_chemical_formula_weight         1384.5
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source
'International Tables for X-ray Crystallography, Vol. IV'
_audit_creation_method           'RAELSPUB and manual entry'
_cell_angle_alpha                86.67(3)
_cell_angle_beta                 66.67(3)
_cell_angle_gamma                83.14(3)
_cell_formula_units_Z            1
_cell_length_a                   9.795(4)
_cell_length_b                   10.472(4)
_cell_length_c                   11.392(4)
_cell_measurement_reflns_used    10
_cell_measurement_temperature    294
_cell_measurement_theta_max      15
_cell_measurement_theta_min      14
_cell_volume                     1065.2(7)
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       ω--2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.021
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3974
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  30min
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    9.022
_exptl_absorpt_correction_T_max  0.45
_exptl_absorpt_correction_T_min  0.20
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(DeMeulenaer & Tompa, 1965)'
_exptl_crystal_density_diffrn    2.16
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             661.0
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.95
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.41
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     130
_refine_ls_number_reflns         3058
_refine_ls_R_factor_gt           0.026
_refine_ls_shift/su_max          0.012
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.0016F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.036
_reflns_number_gt                3058
_reflns_number_total             3731
_reflns_threshold_expression     I>3σ(I)
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '?' to '1'
 for all fully occupied atoms.

 Antanas Vaitkus,
 2017-02-14
;
_cod_original_cell_volume        1065.2(8)
_cod_database_code               4300100
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_type_symbol
_atom_site_occupancy
Cu1 0.50000 0.50000 0.50000 0.0305(2) Uani Cu 1
Cu2 0.14444(5) 0.53578(4) 0.54887(4) 0.0309(1) Uani Cu 1
Br1 0.34062(4) 0.68328(4) 0.46283(4) 0.0372(1) Uani Br 1
Br2 0.14830(6) 0.53307(5) 0.75689(4) 0.0561(2) Uani Br 1
Br3 0.04548(4) 0.61384(4) 0.38856(4) 0.0403(1) Uani Br 1
Br4 0.38083(4) 0.36097(4) 0.41981(4) 0.0367(1) Uani Br 1
P 0.73981(10) 0.16443(9) -0.03050(8) 0.0282(2) Uani P 1
C1 0.7130(3) 0.0630(2) 0.1079(2) 0.0299(8) Uani C 1
C2 0.7193(3) -0.0700(2) 0.1007(2) 0.0354(7) Uani C 1
C3 0.6972(3) -0.1456(2) 0.2094(3) 0.0426(9) Uani C 1
C4 0.6691(3) -0.0890(3) 0.3241(3) 0.0444(9) Uani C 1
C5 0.6626(3) 0.0426(3) 0.3321(2) 0.0427(8) Uani C 1
C6 0.6845(3) 0.1193(2) 0.2242(2) 0.0354(7) Uani C 1
C7 0.5702(3) 0.2625(3) -0.0106(2) 0.0294(7) Uani C 1
C8 0.4402(3) 0.2500(3) 0.0977(2) 0.0349(7) Uani C 1
C9 0.3075(3) 0.3207(3) 0.1067(3) 0.0407(9) Uani C 1
C10 0.3046(3) 0.4031(3) 0.0087(2) 0.0408(8) Uani C 1
C11 0.4328(3) 0.4161(3) -0.0989(3) 0.0396(7) Uani C 1
C12 0.5663(3) 0.3460(3) -0.1092(2) 0.0340(7) Uani C 1
C13 0.7958(3) 0.0665(3) -0.1692(3) 0.0323(9) Uani C 1
C14 0.7008(3) 0.0593(3) -0.2321(3) 0.0384(9) Uani C 1
C15 0.7444(3) -0.0210(3) -0.3360(3) 0.046(1) Uani C 1
C16 0.8816(3) -0.0934(3) -0.3767(3) 0.052(1) Uani C 1
C17 0.9765(3) -0.0870(3) -0.3150(3) 0.057(1) Uani C 1
C18 0.9342(3) -0.0071(3) -0.2110(3) 0.0454(9) Uani C 1
C19 0.8845(4) 0.2630(4) -0.0495(4) 0.0397(9) Uani C 1
HC2 0.73979 -0.11087 0.01743 0.040 Uani H 1
HC3 0.70167 -0.24111 0.20462 0.052 Uani H 1
HC4 0.65315 -0.14388 0.40224 0.053 Uani H 1
HC5 0.64209 0.08273 0.41576 0.052 Uani H 1
HC6 0.67988 0.21477 0.22975 0.039 Uani H 1
HC8 0.44247 0.19015 0.16868 0.040 Uani H 1
HC9 0.21383 0.31191 0.18434 0.050 Uani H 1
HC10 0.20863 0.45387 0.01564 0.047 Uani H 1
HC11 0.42958 0.47615 -0.16950 0.048 Uani H 1
HC12 0.65941 0.35531 -0.18713 0.038 Uani H 1
HC14 0.60131 0.11197 -0.20243 0.047 Uani H 1
HC15 0.67646 -0.02635 -0.38149 0.058 Uani H 1
HC16 0.91263 -0.15123 -0.45177 0.064 Uani H 1
HC17 1.07575 -0.13996 -0.34530 0.079 Uani H 1
HC18 1.00281 -0.00228 -0.16603 0.056 Uani H 1
H1C19 0.90113 0.32032 -0.12626 0.040 Uani H 1
H2C19 0.85428 0.31679 0.02824 0.040 Uani H 1
H3C19 0.97907 0.20710 -0.06126 0.040 Uani H 1
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Cu1 Br4 88.9(1) 1_555 1_555 1_555 no
Br1 Cu1 Br4 91.1(1) 1_555 1_555 2_666 no
Br1 Cu2 Br2 92.8(1) 1_555 1_555 1_555 no
Br1 Cu2 Br3 90.2(1) 1_555 1_555 1_555 no
Br1 Cu2 Br4 81.3(1) 1_555 1_555 1_555 no
Br1 Cu2 Br3 174.2(1) 1_555 1_555 2_566 no
Br2 Cu2 Br3 153.2(1) 1_555 1_555 1_555 no
Br2 Cu2 Br4 102.9(1) 1_555 1_555 1_555 no
Br2 Cu2 Br3 92.9(1) 1_555 1_555 2_566 no
Br3 Cu2 Br4 103.9(1) 1_555 1_555 1_555 no
Br3 Cu2 Br3 85.3(1) 1_555 1_555 2_566 no
Br4 Cu2 Br3 96.2(1) 1_555 1_555 2_566 no
Cu1 Br1 Cu2 83.6(1) 1_555 1_555 1_555 no
Cu2 Br3 Cu2 94.7(1) 1_555 1_555 2_566 no
Cu1 Br4 Cu2 79.2(1) 1_555 1_555 1_555 no
C1 P C7 110.1(1) 1_555 1_555 1_555 no
C1 P C13 109.4(1) 1_555 1_555 1_555 no
C1 P C19 108.3(2) 1_555 1_555 1_555 no
C7 P C13 109.5(1) 1_555 1_555 1_555 no
C7 P C19 110.2(2) 1_555 1_555 1_555 no
C13 P C19 109.3(2) 1_555 1_555 1_555 no
P C1 C2 121.2(2) 1_555 1_555 1_555 no
P C1 C6 119.0(2) 1_555 1_555 1_555 no
C2 C1 C6 119.8(2) 1_555 1_555 1_555 no
C1 C2 C3 119.8(2) 1_555 1_555 1_555 no
C2 C3 C4 120.0(2) 1_555 1_555 1_555 no
C3 C4 C5 120.7(2) 1_555 1_555 1_555 no
C4 C5 C6 120.0(2) 1_555 1_555 1_555 no
C1 C6 C5 119.8(2) 1_555 1_555 1_555 no
P C7 C8 120.9(2) 1_555 1_555 1_555 no
P C7 C12 119.1(2) 1_555 1_555 1_555 no
P C13 C14 121.0(2) 1_555 1_555 1_555 no
P C13 C18 119.2(2) 1_555 1_555 1_555 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 Br1 2.452(1) 1_555 1_555 no
Cu1 Br4 2.392(1) 1_555 1_555 no
Cu1 Br1 2.452(1) 1_555 2_666 no
Cu1 Br4 2.392(1) 1_555 2_666 no
Cu2 Br1 2.466(1) 1_555 1_555 no
Cu2 Br2 2.384(1) 1_555 1_555 no
Cu2 Br3 2.446(1) 1_555 1_555 no
Cu2 Br4 2.734(1) 1_555 1_555 no
Cu2 Br3 2.437(1) 1_555 2_566 no
P C1 1.796(3) 1_555 1_555 no
P C7 1.785(3) 1_555 1_555 no
P C13 1.793(3) 1_555 1_555 no
P C19 1.790(4) 1_555 1_555 no
C1 C2 1.392(2) 1_555 1_555 no
C1 C6 1.392(2) 1_555 1_555 no
C2 C3 1.386(2) 1_555 1_555 no
C3 C4 1.378(2) 1_555 1_555 no
C4 C5 1.378(2) 1_555 1_555 no
C5 C6 1.386(2) 1_555 1_555 no
