#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/80/2218097.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2218097
loop_
_publ_author_name
'Kirillov, Alexander M.'
'Smoleński, Piotr'
'Guedes da Silva, M. Fátima C.'
'Kopylovich, Maximilian N.'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Three-dimensional hydrogen-bonded supramolecular assembly in
 tetrakis(1,3,5-triaza-7-phosphaadamantane)copper(I) chloride
 hexahydrate
;
_journal_coeditor_code           DN2329
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m603
_journal_page_last               m604
_journal_paper_doi               10.1107/S1600536808008179
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Cu (C6 H12 N3 P)4] Cl, 6H2 O'
_chemical_formula_moiety         'C24 H48 Cu N12 P4 +, 24Cl0.04 -, 6H2 O'
_chemical_formula_sum            'C24 H60 Cl Cu N12 O6 P4'
_chemical_formula_weight         835.71
_chemical_name_systematic
;
tetrakis(1,3,5-triaza-7-phosphaadamantane)copper(I) chloride hexahydrate
;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.795(4)
_cell_length_b                   19.795(4)
_cell_length_c                   19.795(4)
_cell_measurement_reflns_used    743
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.91
_cell_volume                     7757(3)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996), PLATON (Spek, 2003) and
Mercury (Macrae et al.,  2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3022
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.9049
_exptl_absorpt_correction_T_min  0.8484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3536
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.320
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     28
_refine_ls_number_reflns         447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0463P)²+19.2954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                361
_reflns_number_total             447
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            dn2329.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_database_code               2218097
_cod_database_fobs_code          2218097
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'z, x, y'
'y, z, x'
'-z+1/4, -x+1/4, y'
'-y+1/4, z, -x+1/4'
'z, -x+1/4, -y+1/4'
'-y+1/4, -z+1/4, x'
'-z+1/4, x, -y+1/4'
'y, -z+1/4, -x+1/4'
'-y, -x, -z'
'y+1/4, x+1/4, -z'
'y+1/4, -x, z+1/4'
'-y, x+1/4, z+1/4'
'-x, -z, -y'
'-z, -y, -x'
'x+1/4, z+1/4, -y'
'-z, y+1/4, x+1/4'
'x+1/4, -z, y+1/4'
'z+1/4, y+1/4, -x'
'-x, z+1/4, y+1/4'
'z+1/4, -y, x+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-z+1/4, -x+3/4, y+1/2'
'-y+1/4, z+1/2, -x+3/4'
'z, -x+3/4, -y+3/4'
'-y+1/4, -z+3/4, x+1/2'
'-z+1/4, x+1/2, -y+3/4'
'y, -z+3/4, -x+3/4'
'-y, -x+1/2, -z+1/2'
'y+1/4, x+3/4, -z+1/2'
'y+1/4, -x+1/2, z+3/4'
'-y, x+3/4, z+3/4'
'-x, -z+1/2, -y+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/4, z+3/4, -y+1/2'
'-z, y+3/4, x+3/4'
'x+1/4, -z+1/2, y+3/4'
'z+1/4, y+3/4, -x+1/2'
'-x, z+3/4, y+3/4'
'z+1/4, -y+1/2, x+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-z+3/4, -x+1/4, y+1/2'
'-y+3/4, z, -x+3/4'
'z+1/2, -x+1/4, -y+3/4'
'-y+3/4, -z+1/4, x+1/2'
'-z+3/4, x, -y+3/4'
'y+1/2, -z+1/4, -x+3/4'
'-y+1/2, -x, -z+1/2'
'y+3/4, x+1/4, -z+1/2'
'y+3/4, -x, z+3/4'
'-y+1/2, x+1/4, z+3/4'
'-x+1/2, -z, -y+1/2'
'-z+1/2, -y, -x+1/2'
'x+3/4, z+1/4, -y+1/2'
'-z+1/2, y+1/4, x+3/4'
'x+3/4, -z, y+3/4'
'z+3/4, y+1/4, -x+1/2'
'-x+1/2, z+1/4, y+3/4'
'z+3/4, -y, x+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-z+3/4, -x+3/4, y'
'-y+3/4, z+1/2, -x+1/4'
'z+1/2, -x+3/4, -y+1/4'
'-y+3/4, -z+3/4, x'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, -z+3/4, -x+1/4'
'-y+1/2, -x+1/2, -z'
'y+3/4, x+3/4, -z'
'y+3/4, -x+1/2, z+1/4'
'-y+1/2, x+3/4, z+1/4'
'-x+1/2, -z+1/2, -y'
'-z+1/2, -y+1/2, -x'
'x+3/4, z+3/4, -y'
'-z+1/2, y+3/4, x+1/4'
'x+3/4, -z+1/2, y+1/4'
'z+3/4, y+3/4, -x'
'-x+1/2, z+3/4, y+1/4'
'z+3/4, -y+1/2, x+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-z, -x, -y'
'-y, -z, -x'
'z-1/4, x-1/4, -y'
'y-1/4, -z, x-1/4'
'-z, x-1/4, y-1/4'
'y-1/4, z-1/4, -x'
'z-1/4, -x, y-1/4'
'-y, z-1/4, x-1/4'
'y, x, z'
'-y-1/4, -x-1/4, z'
'-y-1/4, x, -z-1/4'
'y, -x-1/4, -z-1/4'
'x, z, y'
'z, y, x'
'-x-1/4, -z-1/4, y'
'z, -y-1/4, -x-1/4'
'-x-1/4, z, -y-1/4'
'-z-1/4, -y-1/4, x'
'x, -z-1/4, -y-1/4'
'-z-1/4, y, -x-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'z-1/4, x+1/4, -y+1/2'
'y-1/4, -z+1/2, x+1/4'
'-z, x+1/4, y+1/4'
'y-1/4, z+1/4, -x+1/2'
'z-1/4, -x+1/2, y+1/4'
'-y, z+1/4, x+1/4'
'y, x+1/2, z+1/2'
'-y-1/4, -x+1/4, z+1/2'
'-y-1/4, x+1/2, -z+1/4'
'y, -x+1/4, -z+1/4'
'x, z+1/2, y+1/2'
'z, y+1/2, x+1/2'
'-x-1/4, -z+1/4, y+1/2'
'z, -y+1/4, -x+1/4'
'-x-1/4, z+1/2, -y+1/4'
'-z-1/4, -y+1/4, x+1/2'
'x, -z+1/4, -y+1/4'
'-z-1/4, y+1/2, -x+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'z+1/4, x-1/4, -y+1/2'
'y+1/4, -z, x+1/4'
'-z+1/2, x-1/4, y+1/4'
'y+1/4, z-1/4, -x+1/2'
'z+1/4, -x, y+1/4'
'-y+1/2, z-1/4, x+1/4'
'y+1/2, x, z+1/2'
'-y+1/4, -x-1/4, z+1/2'
'-y+1/4, x, -z+1/4'
'y+1/2, -x-1/4, -z+1/4'
'x+1/2, z, y+1/2'
'z+1/2, y, x+1/2'
'-x+1/4, -z-1/4, y+1/2'
'z+1/2, -y-1/4, -x+1/4'
'-x+1/4, z, -y+1/4'
'-z+1/4, -y-1/4, x+1/2'
'x+1/2, -z-1/4, -y+1/4'
'-z+1/4, y, -x+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'z+1/4, x+1/4, -y'
'y+1/4, -z+1/2, x-1/4'
'-z+1/2, x+1/4, y-1/4'
'y+1/4, z+1/4, -x'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, z+1/4, x-1/4'
'y+1/2, x+1/2, z'
'-y+1/4, -x+1/4, z'
'-y+1/4, x+1/2, -z-1/4'
'y+1/2, -x+1/4, -z-1/4'
'x+1/2, z+1/2, y'
'z+1/2, y+1/2, x'
'-x+1/4, -z+1/4, y'
'z+1/2, -y+1/4, -x-1/4'
'-x+1/4, z+1/2, -y-1/4'
'-z+1/4, -y+1/4, x'
'x+1/2, -z+1/4, -y-1/4'
'-z+1/4, y+1/2, -x-1/4'
loop_
_atom_site_type_symbol
_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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.25075(10) 0.15137(15) 0.25075(10) 0.0199(6) Uani d S 1
H H1A 0.2258 0.1228 0.2818 0.024 Uiso calc PR 0.50
H H1B 0.2818 0.1228 0.2258 0.024 Uiso calc PR 0.50
C C2 0.33080(15) 0.24509(11) 0.24509(11) 0.0239(7) Uani d S 1
H H2A 0.3607 0.2726 0.2726 0.029 Uiso calc SR 1
H H2B 0.3587 0.2166 0.2166 0.029 Uiso calc SR 1
N N1 0.29002(8) 0.20160(12) 0.29002(8) 0.0212(6) Uani d S 1
Cu Cu1 0.1250 0.1250 0.1250 0.0134(3) Uani d S 1
P P1 0.19090(4) 0.19090(4) 0.19090(4) 0.0156(3) Uani d S 1
Cl Cl1 0.3750 0.3750 0.3750 0.0165(5) Uani d S 1
O O10 0.3750 0.12300(14) 0.3750 0.0240(7) Uani d S 1
H H10 0.3521 0.1480 0.3521 0.036 Uiso d SR 1
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'
Cu Cu 0.3201 1.2651 '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'
Cl Cl 0.1484 0.1585 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 P1 . . 112.8(2)
N1 C1 H1A . . 109.0
P1 C1 H1B . . 109.0
H1A C1 H1B . . 107.8
N1 C2 N1 5 . 113.7(3)
N1 C2 H2A . . 108.8
N1 C2 H2B . . 108.8
H2A C2 H2B . . 107.7
C2 N1 C2 6 . 108.5(3)
C2 N1 C1 6 . 111.21(16)
C2 N1 C1 . . 111.21(16)
P1 Cu1 P1 . 4 109.5
P1 Cu1 P1 . 2 109.5
P1 Cu1 P1 4 2 109.5
P1 Cu1 P1 . 3 109.5
P1 Cu1 P1 4 3 109.5
P1 Cu1 P1 2 3 109.5
C1 P1 C1 6 5 97.57(12)
C1 P1 C1 6 . 97.57(12)
C1 P1 C1 5 . 97.57(12)
C1 P1 Cu1 6 . 119.70(9)
C1 P1 Cu1 5 . 119.70(9)
C1 P1 Cu1 . . 119.70(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.482(3)
C1 P1 . 1.849(3)
C1 H1A . 0.9700
C1 H1B . 0.9700
C2 N1 5 1.478(2)
C2 N1 . 1.478(2)
C2 H2A . 0.9700
C2 H2B . 0.9700
Cu1 P1 . 2.2596(13)
P1 C1 5 1.849(3)
O10 H10 . 0.8104
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O10 H10 N1 0.81 2.04 2.843(3) 173.8
