#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:53:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179904 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/00/7020045.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_7020045
loop_
_publ_author_name
'Williams, Edward R.'
'Morris, Samuel A.'
'Weller, Mark T.'
_publ_section_title
;
 Copper(ii) fluorophosphates.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10845
_journal_page_last               10853
_journal_paper_doi               10.1039/c2dt31131c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C6 H16 Cu3 F4 N2 O12 P4'
_chemical_formula_weight         672.68
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-05-11 # Formatted by publCIF
;
_cell_angle_alpha                90.428(2)
_cell_angle_beta                 94.283(2)
_cell_angle_gamma                99.977(2)
_cell_formula_units_Z            2
_cell_length_a                   5.7913(2)
_cell_length_b                   9.6085(3)
_cell_length_c                   16.3303(5)
_cell_measurement_reflns_used    11458
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     892.28(5)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0977
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15742
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    4.011
_exptl_absorpt_correction_T_max  0.8246
_exptl_absorpt_correction_T_min  0.6898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.601
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.274
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4108
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0719
_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)+(0.0000P)²+19.9405P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1381
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                2960
_reflns_number_total             4108
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c2dt31131c.txt
_cod_data_source_block           test1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7020045
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
F1 F 0.5802(9) 0.6673(5) 0.2684(3) 0.0162(11) Uani 1 1 d .
F2 F 0.6579(9) 0.6996(5) 0.5689(3) 0.0163(11) Uani 1 1 d .
F3 F 1.1319(9) 0.7224(5) 0.1095(3) 0.0149(10) Uani 1 1 d .
O4 O 0.7648(10) 0.8736(6) 0.4663(3) 0.0095(11) Uani 1 1 d .
O5 O 1.1660(10) 0.9753(6) 0.1473(3) 0.0131(12) Uani 1 1 d .
F6 F 0.8421(9) 1.3701(5) 0.2268(3) 0.0187(11) Uani 1 1 d .
O7 O 0.8872(10) 0.8632(6) 0.0298(3) 0.0101(11) Uani 1 1 d .
O8 O 0.6142(10) 0.8390(6) 0.1601(3) 0.0133(12) Uani 1 1 d .
O9 O 0.6074(10) 1.1325(6) 0.4622(3) 0.0108(12) Uani 1 1 d .
O10 O 1.0927(11) 1.1934(6) 0.2413(3) 0.0149(13) Uani 1 1 d .
O11 O 1.2045(11) 1.0538(6) 0.3849(3) 0.0138(13) Uani 1 1 d .
O12 O 0.6757(10) 1.1019(6) -0.0173(4) 0.0139(12) Uani 1 1 d .
O13 O 0.8270(10) 0.8955(6) 0.3005(3) 0.0130(12) Uani 1 1 d .
O14 O 0.3877(10) 0.8669(6) 0.2863(3) 0.0123(12) Uani 1 1 d .
O15 O 0.7040(12) 1.1610(7) 0.3059(4) 0.0220(15) Uani 1 1 d .
O16 O 0.7095(11) 1.1508(6) 0.1518(4) 0.0172(13) Uani 1 1 d .
N2 N 0.6616(12) 0.7086(7) 0.8972(4) 0.0127(14) Uiso 1 1 d .
H2A H 0.7634 0.7442 0.8614 0.019 Uiso 1 1 calc R
H2B H 0.7161 0.7403 0.9476 0.019 Uiso 1 1 calc R
H2C H 0.5239 0.7353 0.8845 0.019 Uiso 1 1 calc R
N1 N 0.1128(12) 0.7256(7) 0.4048(4) 0.0102(13) Uiso 1 1 d .
H1A H 0.1940 0.7679 0.3650 0.015 Uiso 1 1 calc R
H1B H 0.1933 0.7476 0.4531 0.015 Uiso 1 1 calc R
H1C H -0.0252 0.7545 0.4046 0.015 Uiso 1 1 calc R
C1 C 0.0734(16) 0.5698(9) 0.3910(5) 0.0158(18) Uiso 1 1 d .
H6A H 0.2241 0.5389 0.3905 0.019 Uiso 1 1 calc R
H6B H -0.0111 0.5464 0.3378 0.019 Uiso 1 1 calc R
C2 C -0.0664(15) 0.4917(9) 0.4574(5) 0.0146(17) Uiso 1 1 d .
H7A H -0.1049 0.3921 0.4424 0.017 Uiso 1 1 calc R
H7B H -0.2128 0.5271 0.4598 0.017 Uiso 1 1 calc R
C4 C 0.6300(16) 0.5493(9) 0.8943(5) 0.0173(18) Uiso 1 1 d .
H4A H 0.7805 0.5204 0.9076 0.021 Uiso 1 1 calc R
H4B H 0.5738 0.5150 0.8391 0.021 Uiso 1 1 calc R
C3 C 0.4550(16) 0.4838(10) 0.9548(5) 0.0188(19) Uiso 1 1 d .
H3A H 0.4217 0.3822 0.9457 0.023 Uiso 1 1 calc R
H3B H 0.3089 0.5192 0.9439 0.023 Uiso 1 1 calc R
Cu1 Cu 0.74986(18) 1.02212(11) 0.38684(6) 0.0109(2) Uani 1 1 d .
Cu2 Cu 0.67995(18) 0.98236(11) 0.07917(6) 0.0110(2) Uani 1 1 d .
Cu3 Cu 1.20818(18) 1.01799(11) 0.26454(6) 0.0105(2) Uani 1 1 d .
P4 P 0.6027(4) 0.8280(2) 0.25091(12) 0.0093(4) Uani 1 1 d .
P5 P 0.6526(4) 0.8573(2) 0.54702(12) 0.0103(4) Uani 1 1 d .
P6 P 0.8371(4) 1.2064(2) 0.23220(13) 0.0111(4) Uani 1 1 d .
P7 P 1.1261(4) 0.8735(2) 0.07595(12) 0.0093(4) Uani 1 1 d .
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'
P P 0.1023 0.0942 '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'
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
P5 O4 Cu1 127.6(4) . .
P7 O5 Cu3 151.8(4) . .
P7 O7 Cu2 113.7(3) . .
P4 O8 Cu2 139.1(4) . .
P5 O9 Cu1 122.4(3) 2_676 .
P6 O10 Cu3 124.5(4) . .
P5 O11 Cu3 139.6(4) 2_776 .
P7 O12 Cu2 123.7(3) 2_775 .
P7 O12 Cu2 114.1(3) 2_775 2_675
Cu2 O12 Cu2 101.5(2) . 2_675
P4 O13 Cu1 109.5(3) . .
P4 O13 Cu3 133.9(3) . .
Cu1 O13 Cu3 102.2(2) . .
P4 O14 Cu3 133.3(3) . 1_455
P6 O15 Cu1 130.5(4) . .
P6 O16 Cu2 138.4(4) . .
C4 N2 H2A 109.5 . .
C4 N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
C4 N2 H2C 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
C1 N1 H1A 109.5 . .
C1 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C1 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
N1 C1 C2 111.7(7) . .
N1 C1 H6A 109.3 . .
C2 C1 H6A 109.3 . .
N1 C1 H6B 109.3 . .
C2 C1 H6B 109.3 . .
H6A C1 H6B 107.9 . .
C1 C2 C2 113.1(9) . 2_566
C1 C2 H7A 109.0 . .
C2 C2 H7A 109.0 2_566 .
C1 C2 H7B 109.0 . .
C2 C2 H7B 109.0 2_566 .
H7A C2 H7B 107.8 . .
N2 C4 C3 111.2(7) . .
N2 C4 H4A 109.4 . .
C3 C4 H4A 109.4 . .
N2 C4 H4B 109.4 . .
C3 C4 H4B 109.4 . .
H4A C4 H4B 108.0 . .
C4 C3 C3 113.1(9) . 2_667
C4 C3 H3A 109.0 . .
C3 C3 H3A 109.0 2_667 .
C4 C3 H3B 109.0 . .
C3 C3 H3B 109.0 2_667 .
H3A C3 H3B 107.8 . .
O15 Cu1 O9 87.1(3) . .
O15 Cu1 O4 174.5(3) . .
O9 Cu1 O4 92.0(2) . .
O15 Cu1 O13 90.3(3) . .
O9 Cu1 O13 168.0(2) . .
O4 Cu1 O13 89.5(2) . .
O15 Cu1 P4 83.2(2) . .
O9 Cu1 P4 138.13(17) . .
O4 Cu1 P4 93.95(17) . .
O13 Cu1 P4 29.92(17) . .
O8 Cu2 O12 165.7(2) . .
O8 Cu2 O16 98.6(3) . .
O12 Cu2 O16 90.1(3) . .
O8 Cu2 O7 88.1(2) . .
O12 Cu2 O7 92.7(2) . .
O16 Cu2 O7 139.0(2) . .
O8 Cu2 O12 87.4(2) . 2_675
O12 Cu2 O12 78.5(2) . 2_675
O16 Cu2 O12 117.5(3) . 2_675
O7 Cu2 O12 103.1(2) . 2_675
O5 Cu3 O14 92.9(2) . 1_655
O5 Cu3 O10 87.9(2) . .
O14 Cu3 O10 168.1(3) 1_655 .
O5 Cu3 O11 172.3(3) . .
O14 Cu3 O11 90.3(2) 1_655 .
O10 Cu3 O11 90.5(2) . .
O5 Cu3 O13 97.7(2) . .
O14 Cu3 O13 98.5(2) 1_655 .
O10 Cu3 O13 93.2(2) . .
O11 Cu3 O13 74.9(2) . .
O8 P4 O14 116.8(3) . .
O8 P4 O13 114.3(3) . .
O14 P4 O13 111.3(3) . .
O8 P4 F1 105.2(3) . .
O14 P4 F1 103.1(3) . .
O13 P4 F1 104.4(3) . .
O8 P4 Cu1 133.9(2) . .
O14 P4 Cu1 70.9(2) . .
O13 P4 Cu1 40.6(2) . .
F1 P4 Cu1 117.4(2) . .
O11 P5 O4 112.8(3) 2_776 .
O11 P5 O9 115.6(4) 2_776 2_676
O4 P5 O9 112.3(3) . 2_676
O11 P5 F2 106.7(3) 2_776 .
O4 P5 F2 103.4(3) . .
O9 P5 F2 104.8(3) 2_676 .
O10 P6 O16 114.8(4) . .
O10 P6 O15 114.4(4) . .
O16 P6 O15 113.8(4) . .
O10 P6 F6 103.8(3) . .
O16 P6 F6 102.9(3) . .
O15 P6 F6 105.4(4) . .
O5 P7 O7 113.9(3) . .
O5 P7 O12 113.1(3) . 2_775
O7 P7 O12 111.4(3) . 2_775
O5 P7 F3 108.1(3) . .
O7 P7 F3 105.0(3) . .
O12 P7 F3 104.5(3) 2_775 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
F1 P4 1.557(5) .
F2 P5 1.564(5) .
F3 P7 1.560(5) .
O4 P5 1.510(6) .
O4 Cu1 1.944(5) .
O5 P7 1.495(6) .
O5 Cu3 1.943(6) .
F6 P6 1.571(5) .
O7 P7 1.513(6) .
O7 Cu2 2.002(6) .
O8 P4 1.494(6) .
O8 Cu2 1.926(6) .
O9 P5 1.522(6) 2_676
O9 Cu1 1.938(6) .
O10 P6 1.503(7) .
O10 Cu3 1.948(6) .
O11 P5 1.501(6) 2_776
O11 Cu3 1.995(6) .
O12 P7 1.537(6) 2_775
O12 Cu2 1.958(6) .
O12 Cu2 2.240(6) 2_675
O13 P4 1.519(6) .
O13 Cu1 1.981(6) .
O13 Cu3 2.431(6) .
O14 P4 1.514(6) .
O14 Cu3 1.947(6) 1_455
O15 P6 1.505(6) .
O15 Cu1 1.922(6) .
O16 P6 1.505(6) .
O16 Cu2 1.975(6) .
N2 C4 1.510(11) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N1 C1 1.487(11) .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
N1 H1C 0.8900 .
C1 C2 1.525(12) .
C1 H6A 0.9700 .
C1 H6B 0.9700 .
C2 C2 1.532(16) 2_566
C2 H7A 0.9700 .
C2 H7B 0.9700 .
C4 C3 1.528(12) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C3 C3 1.540(17) 2_667
C3 H3A 0.9700 .
C3 H3B 0.9700 .
Cu1 P4 2.870(2) .
Cu2 O12 2.240(6) 2_675
Cu3 O14 1.947(6) 1_655
P5 O11 1.501(6) 2_776
P5 O9 1.522(6) 2_676
P7 O12 1.537(6) 2_775
