#------------------------------------------------------------------------------
#$Date: 2017-05-05 06:19:20 +0300 (Fri, 05 May 2017) $
#$Revision: 196214 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/00/7120079.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_7120079
loop_
_publ_author_name
'Keyzer, Evan N.'
'Matthews, Peter D.'
'Liu, Zigeng'
'Bond, Andrew D.'
'Grey, Clare P.'
'Wright, Dominic S.'
_publ_section_title
;
 Synthesis of Ca(PF6)2, formed via nitrosonium oxidation of calcium.
;
_journal_issue                   33
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4573
_journal_page_last               4576
_journal_paper_doi               10.1039/c7cc01938f
_journal_volume                  53
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C8 H12 Ca F2 N4 O2 P +, F6 P -'
_chemical_formula_sum            'C8 H12 Ca F8 N4 O2 P2'
_chemical_formula_weight         450.24
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-26 deposited with the CCDC.
2017-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9151(14)
_cell_length_b                   20.3651(14)
_cell_length_c                   7.0543(6)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.57
_cell_measurement_theta_min      4.05
_cell_volume                     1855.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       'ω and φ-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11439
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.551
_diffrn_reflns_theta_max         66.551
_diffrn_reflns_theta_min         4.053
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    5.405
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       needle
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1669
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0695P)²+4.5812P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                1644
_reflns_number_total             1669
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc01938f2.cif
_cod_data_source_block           DW_B1_0029
_cod_database_code               7120079
_cambridge_user_name             'Evan Keyzer'
_cambridge_user_crsid            ek406
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             enk-2-8
_cambridge_data_id               DW_B1_0029
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.397
_shelx_estimated_absorpt_t_max   0.737
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ca1 Ca 0.5000 0.55111(5) 0.90444(19) 0.0198(3) Uani 1 2 d S T P
P1 P 0.5000 0.60526(7) 0.4076(3) 0.0249(4) Uani 1 2 d S T P
O1 O 0.5000 0.5622(3) 0.5743(7) 0.0246(11) Uani 1 2 d S T P
O2 O 0.5000 0.5722(3) 0.2240(8) 0.0327(12) Uani 1 2 d S T P
F1 F 0.5902(3) 0.65337(16) 0.4186(7) 0.0577(10) Uani 1 1 d . . .
N1 N 0.6152(4) 0.6513(2) 0.8945(9) 0.0456(12) Uani 1 1 d . . .
N2 N 0.3177(3) 0.5074(2) 0.8652(7) 0.0366(12) Uani 1 1 d . . .
C1 C 0.6508(5) 0.7011(3) 0.8626(8) 0.0385(14) Uani 1 1 d . . .
C2 C 0.6942(7) 0.7658(3) 0.8219(13) 0.063(2) Uani 1 1 d . . .
H2A H 0.6692 0.7810 0.6983 0.095 Uiso 1 1 calc R U .
H2B H 0.7700 0.7630 0.8195 0.095 Uiso 1 1 calc R U .
H2C H 0.6727 0.7968 0.9204 0.095 Uiso 1 1 calc R U .
C3 C 0.2449(4) 0.4836(3) 0.8142(9) 0.0351(12) Uani 1 1 d . . .
C4 C 0.1506(5) 0.4521(4) 0.7444(12) 0.0557(18) Uani 1 1 d . . .
H4A H 0.0975 0.4855 0.7213 0.083 Uiso 1 1 calc R U .
H4B H 0.1254 0.4207 0.8391 0.083 Uiso 1 1 calc R U .
H4C H 0.1657 0.4288 0.6259 0.083 Uiso 1 1 calc R U .
P2 P 0.0000 0.35104(10) 0.2823(3) 0.0389(5) Uani 1 2 d S T P
F2 F 0.0000 0.4191(3) 0.3918(16) 0.094(2) Uani 1 2 d S T P
F3 F 0.0000 0.2839(4) 0.1803(16) 0.126(4) Uani 1 2 d S T P
F4 F 0.1132(6) 0.3499(6) 0.296(2) 0.251(9) Uani 1 1 d . . .
F5 F 0.0000 0.3834(7) 0.0956(19) 0.221(9) Uani 1 2 d S T P
F6 F 0.0000 0.3199(8) 0.4750(19) 0.247(12) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
O2 Ca1 O1 163.64(18) 1_556 .
O2 Ca1 N1 82.9(2) 1_556 4_655
O1 Ca1 N1 83.93(19) . 4_655
O2 Ca1 N1 82.9(2) 1_556 .
O1 Ca1 N1 83.93(19) . .
N1 Ca1 N1 72.2(2) 4_655 .
O2 Ca1 N2 99.98(12) 1_556 4_655
O1 Ca1 N2 85.71(12) . 4_655
N1 Ca1 N2 145.94(18) 4_655 4_655
N1 Ca1 N2 74.52(16) . 4_655
O2 Ca1 N2 99.98(12) 1_556 .
O1 Ca1 N2 85.71(12) . .
N1 Ca1 N2 74.52(16) 4_655 .
N1 Ca1 N2 145.94(17) . .
N2 Ca1 N2 136.8(2) 4_655 .
O2 Ca1 O1 73.37(18) 1_556 2_665
O1 Ca1 O1 122.99(14) . 2_665
N1 Ca1 O1 136.85(16) 4_655 2_665
N1 Ca1 O1 136.85(16) . 2_665
N2 Ca1 O1 74.84(11) 4_655 2_665
N2 Ca1 O1 74.84(11) . 2_665
O2 Ca1 O2 127.68(16) 1_556 2_665
O1 Ca1 O2 68.68(16) . 2_665
N1 Ca1 O2 135.06(15) 4_655 2_665
N1 Ca1 O2 135.06(15) . 2_665
N2 Ca1 O2 68.73(11) 4_655 2_665
N2 Ca1 O2 68.72(11) . 2_665
O1 Ca1 O2 54.31(13) 2_665 2_665
O2 Ca1 P1 100.40(16) 1_556 2_665
O1 Ca1 P1 95.96(14) . 2_665
N1 Ca1 P1 143.88(12) 4_655 2_665
N1 Ca1 P1 143.88(12) . 2_665
N2 Ca1 P1 69.48(11) 4_655 2_665
N2 Ca1 P1 69.47(11) . 2_665
O1 Ca1 P1 27.03(12) 2_665 2_665
O2 Ca1 P1 27.28(13) 2_665 2_665
O2 Ca1 Ca1 41.35(15) 1_556 2_665
O1 Ca1 Ca1 155.01(14) . 2_665
N1 Ca1 Ca1 115.74(16) 4_655 2_665
N1 Ca1 Ca1 115.74(16) . 2_665
N2 Ca1 Ca1 85.16(11) 4_655 2_665
N2 Ca1 Ca1 85.16(11) . 2_665
O1 Ca1 Ca1 32.02(12) 2_665 2_665
O2 Ca1 Ca1 86.33(13) 2_665 2_665
P1 Ca1 Ca1 59.05(5) 2_665 2_665
O2 Ca1 Ca1 160.26(16) 1_556 2_664
O1 Ca1 Ca1 36.10(13) . 2_664
N1 Ca1 Ca1 112.75(15) 4_655 2_664
N1 Ca1 Ca1 112.75(15) . 2_664
N2 Ca1 Ca1 74.17(12) 4_655 2_664
N2 Ca1 Ca1 74.17(12) . 2_664
O1 Ca1 Ca1 86.89(12) 2_665 2_664
O2 Ca1 Ca1 32.58(12) 2_665 2_664
P1 Ca1 Ca1 59.86(5) 2_665 2_664
Ca1 Ca1 Ca1 118.91(5) 2_665 2_664
O2 P1 O1 115.9(3) . .
O2 P1 F1 110.0(2) . .
O1 P1 F1 110.1(2) . .
O2 P1 F1 110.0(2) . 4_655
O1 P1 F1 110.1(2) . 4_655
F1 P1 F1 99.7(3) . 4_655
O2 P1 Ca1 62.2(2) . 2_664
O1 P1 Ca1 53.7(2) . 2_664
F1 P1 Ca1 130.03(17) . 2_664
F1 P1 Ca1 130.04(17) 4_655 2_664
P1 O1 Ca1 148.9(3) . .
P1 O1 Ca1 99.3(3) . 2_664
Ca1 O1 Ca1 111.9(2) . 2_664
P1 O2 Ca1 163.4(4) . 1_554
P1 O2 Ca1 90.6(3) . 2_664
Ca1 O2 Ca1 106.1(2) 1_554 2_664
C1 N1 Ca1 164.8(6) . .
C3 N2 Ca1 165.9(5) . .
N1 C1 C2 178.7(7) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N2 C3 C4 179.0(7) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
F4 P2 F4 172.4(14) . 4
F4 P2 F5 93.7(7) . .
F4 P2 F5 93.7(7) 4 .
F4 P2 F6 86.3(7) . .
F4 P2 F6 86.3(7) 4 .
F5 P2 F6 178.5(9) . .
F4 P2 F3 90.9(4) . .
F4 P2 F3 90.9(4) 4 .
F5 P2 F3 88.8(7) . .
F6 P2 F3 92.7(8) . .
F4 P2 F2 89.0(4) . .
F4 P2 F2 89.0(4) 4 .
F5 P2 F2 92.6(8) . .
F6 P2 F2 85.9(8) . .
F3 P2 F2 178.6(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 O2 2.295(6) 1_556
Ca1 O1 2.340(5) .
Ca1 N1 2.525(4) 4_655
Ca1 N1 2.525(4) .
Ca1 N2 2.532(4) 4_655
Ca1 N2 2.532(4) .
Ca1 O1 2.601(5) 2_665
Ca1 O2 2.816(6) 2_665
Ca1 P1 3.1844(18) 2_665
Ca1 Ca1 4.0955(11) 2_665
Ca1 Ca1 4.0955(11) 2_664
P1 O2 1.460(6) .
P1 O1 1.466(6) .
P1 F1 1.524(3) .
P1 F1 1.524(3) 4_655
P1 Ca1 3.1844(18) 2_664
O1 Ca1 2.600(5) 2_664
O2 Ca1 2.295(6) 1_554
O2 Ca1 2.816(6) 2_664
N1 C1 1.138(7) .
N2 C3 1.117(7) .
C1 C2 1.460(8) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.463(8) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
P2 F4 1.465(7) .
P2 F4 1.465(7) 4
P2 F5 1.473(12) .
P2 F6 1.500(13) .
P2 F3 1.545(8) .
P2 F2 1.586(7) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 P1 O1 Ca1 180.000(2) . .
F1 P1 O1 Ca1 54.5(2) . .
F1 P1 O1 Ca1 -54.5(2) 4_655 .
Ca1 P1 O1 Ca1 180.000(4) 2_664 .
O2 P1 O1 Ca1 0.000(1) . 2_664
F1 P1 O1 Ca1 -125.5(2) . 2_664
F1 P1 O1 Ca1 125.5(2) 4_655 2_664
O1 P1 O2 Ca1 180.000(5) . 1_554
F1 P1 O2 Ca1 -54.40(19) . 1_554
F1 P1 O2 Ca1 54.40(19) 4_655 1_554
Ca1 P1 O2 Ca1 180.000(7) 2_664 1_554
O1 P1 O2 Ca1 0.000(1) . 2_664
F1 P1 O2 Ca1 125.60(19) . 2_664
F1 P1 O2 Ca1 -125.60(19) 4_655 2_664
