#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/22/7102275.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_7102275
loop_
_publ_author_name
'Davidson, Reagan J'
'Weigand, Jan J'
'Burford, Neil'
'Cameron, T Stanley'
'Decken, Andreas'
'Werner-Zwanziger, Ulrike'
_publ_section_title
;
 Bifunctional diphosphorus Lewis acids from cyclodiphosphadiazanes.
;
_journal_issue                   44
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4671
_journal_page_last               4673
_journal_paper_doi               10.1039/b710853b
_journal_year                    2007
_chemical_formula_sum            'C18 H18 F6 N2 O6 P2 S2'
_chemical_formula_weight         598.40
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.012(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.985(4)
_cell_length_b                   10.925(3)
_cell_length_c                   18.101(6)
_cell_measurement_reflns_used    7385
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.44
_cell_volume                     2564.2(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17263
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              K760
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.9039
_exptl_absorpt_correction_T_min  0.8361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997b)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Irregular
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         5721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0497P)²+2.5154P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                4520
_reflns_number_total             5721
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            b710853b.txt
_cod_data_source_block           nb070148
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7102275
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
P1 P 0.82444(4) 0.78979(5) 0.13066(3) 0.03150(15) Uani 1 1 d .
P2 P 0.82356(4) 0.94978(5) 0.02763(3) 0.02891(14) Uani 1 1 d .
S1 S 0.66131(6) 0.67004(7) 0.20967(4) 0.0547(2) Uani 1 1 d .
S2 S 0.66600(6) 1.07210(8) -0.06488(4) 0.0566(2) Uani 1 1 d .
N1 N 0.81819(14) 0.79526(17) 0.03644(10) 0.0317(4) Uani 1 1 d .
N2 N 0.81150(13) 0.94388(16) 0.12049(10) 0.0284(4) Uani 1 1 d .
C1 C 0.84604(19) 0.7054(2) -0.01746(13) 0.0364(5) Uani 1 1 d .
C2 C 0.9502(2) 0.6773(2) -0.02446(15) 0.0442(6) Uani 1 1 d .
C3 C 0.9743(3) 0.5951(3) -0.07983(18) 0.0599(8) Uani 1 1 d .
H3 H 1.0444 0.5748 -0.0863 0.072 Uiso 1 1 calc R
C4 C 0.8975(3) 0.5427(3) -0.12554(17) 0.0676(10) Uani 1 1 d .
H4 H 0.9154 0.4874 -0.1633 0.081 Uiso 1 1 calc R
C5 C 0.7959(3) 0.5700(3) -0.11669(17) 0.0635(9) Uani 1 1 d .
H5 H 0.7441 0.5320 -0.1478 0.076 Uiso 1 1 calc R
C6 C 0.7673(2) 0.6528(3) -0.06270(15) 0.0485(6) Uani 1 1 d .
C7 C 1.0339(2) 0.7340(3) 0.02523(19) 0.0564(8) Uani 1 1 d .
H7A H 1.1011 0.7015 0.0125 0.085 Uiso 1 1 calc R
H7B H 1.0219 0.7142 0.0769 0.085 Uiso 1 1 calc R
H7C H 1.0332 0.8230 0.0187 0.085 Uiso 1 1 calc R
C8 C 0.6551(2) 0.6835(3) -0.05577(19) 0.0647(9) Uani 1 1 d .
H8A H 0.6345 0.7468 -0.0919 0.097 Uiso 1 1 calc R
H8B H 0.6446 0.7136 -0.0057 0.097 Uiso 1 1 calc R
H8C H 0.6132 0.6099 -0.0652 0.097 Uiso 1 1 calc R
C9 C 0.82409(16) 1.0453(2) 0.17111(11) 0.0287(4) Uani 1 1 d .
C10 C 0.73712(18) 1.0905(2) 0.20451(12) 0.0344(5) Uani 1 1 d .
C11 C 0.7495(2) 1.1932(2) 0.24958(14) 0.0438(6) Uani 1 1 d .
H11 H 0.6919 1.2249 0.2735 0.053 Uiso 1 1 calc R
C12 C 0.8439(2) 1.2498(3) 0.26005(15) 0.0501(7) Uani 1 1 d .
H12 H 0.8505 1.3210 0.2901 0.060 Uiso 1 1 calc R
C13 C 0.9294(2) 1.2034(2) 0.22698(14) 0.0445(6) Uani 1 1 d .
H13 H 0.9942 1.2431 0.2347 0.053 Uiso 1 1 calc R
C14 C 0.92163(17) 1.0992(2) 0.18248(12) 0.0328(5) Uani 1 1 d .
C15 C 0.63215(19) 1.0319(3) 0.19332(16) 0.0478(6) Uani 1 1 d .
H15A H 0.6257 0.9655 0.2292 0.072 Uiso 1 1 calc R
H15B H 0.6240 0.9987 0.1430 0.072 Uiso 1 1 calc R
H15C H 0.5786 1.0933 0.2005 0.072 Uiso 1 1 calc R
C16 C 1.01647(18) 1.0479(3) 0.14928(15) 0.0449(6) Uani 1 1 d .
H16A H 1.0106 1.0579 0.0954 0.067 Uiso 1 1 calc R
H16B H 1.0229 0.9608 0.1615 0.067 Uiso 1 1 calc R
H16C H 1.0776 1.0918 0.1693 0.067 Uiso 1 1 calc R
C17 C 0.6413(3) 0.5246(3) 0.1637(3) 0.0758(10) Uani 1 1 d .
C18 C 0.6352(3) 1.2068(4) -0.0102(3) 0.0807(12) Uani 1 1 d .
F1 F 0.5721(3) 0.5334(3) 0.10946(18) 0.1362(13) Uani 1 1 d .
F2 F 0.6110(2) 0.4430(2) 0.21199(17) 0.1083(9) Uani 1 1 d .
F3 F 0.7287(3) 0.4884(2) 0.1376(2) 0.1388(13) Uani 1 1 d .
F4 F 0.6131(3) 1.2992(3) -0.05521(19) 0.1348(12) Uani 1 1 d .
F5 F 0.7156(2) 1.2364(2) 0.03460(15) 0.0977(8) Uani 1 1 d .
F6 F 0.5565(2) 1.1860(3) 0.0294(2) 0.1537(15) Uani 1 1 d .
O1 O 0.69671(13) 0.74701(16) 0.14349(10) 0.0425(4) Uani 1 1 d .
O2 O 0.7425(2) 0.6553(3) 0.26362(14) 0.1061(12) Uani 1 1 d .
O3 O 0.5635(2) 0.7093(3) 0.2282(2) 0.1069(12) Uani 1 1 d .
O4 O 0.69569(12) 0.98269(16) -0.00071(10) 0.0406(4) Uani 1 1 d .
O5 O 0.5744(3) 1.0316(3) -0.1007(2) 0.1289(15) Uani 1 1 d .
O6 O 0.75304(19) 1.1045(2) -0.10406(12) 0.0705(7) 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'
S S 0.1246 0.1234 '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
N2 P1 N1 81.82(9)
N2 P1 O1 100.94(9)
N1 P1 O1 98.42(9)
N2 P1 P2 41.19(6)
N1 P1 P2 41.20(7)
O1 P1 P2 108.15(6)
N1 P2 N2 82.11(9)
N1 P2 O4 100.89(9)
N2 P2 O4 99.36(9)
N1 P2 P1 41.40(6)
N2 P2 P1 41.28(6)
O4 P2 P1 108.81(6)
O3 S1 O2 121.7(2)
O3 S1 O1 109.18(15)
O2 S1 O1 110.84(13)
O3 S1 C17 105.6(2)
O2 S1 C17 107.7(2)
O1 S1 C17 99.33(16)
O5 S2 O6 122.1(2)
O5 S2 O4 108.67(15)
O6 S2 O4 111.13(12)
O5 S2 C18 107.5(2)
O6 S2 C18 105.90(17)
O4 S2 C18 98.87(15)
C1 N1 P2 126.86(16)
C1 N1 P1 130.70(16)
P2 N1 P1 97.41(10)
C9 N2 P2 125.94(14)
C9 N2 P1 133.20(14)
P2 N2 P1 97.53(9)
C2 C1 C6 122.5(2)
C2 C1 N1 119.2(2)
C6 C1 N1 118.3(2)
C3 C2 C1 117.4(3)
C3 C2 C7 120.8(3)
C1 C2 C7 121.8(2)
C4 C3 C2 120.9(3)
C4 C3 H3 119.5
C2 C3 H3 119.5
C5 C4 C3 120.5(3)
C5 C4 H4 119.8
C3 C4 H4 119.8
C4 C5 C6 121.1(3)
C4 C5 H5 119.4
C6 C5 H5 119.4
C5 C6 C1 117.5(3)
C5 C6 C8 119.8(3)
C1 C6 C8 122.7(2)
C2 C7 H7A 109.5
C2 C7 H7B 109.5
H7A C7 H7B 109.5
C2 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
C6 C8 H8A 109.5
C6 C8 H8B 109.5
H8A C8 H8B 109.5
C6 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
C10 C9 C14 122.1(2)
C10 C9 N2 118.63(19)
C14 C9 N2 119.19(19)
C11 C10 C9 117.8(2)
C11 C10 C15 119.8(2)
C9 C10 C15 122.4(2)
C12 C11 C10 121.2(2)
C12 C11 H11 119.4
C10 C11 H11 119.4
C11 C12 C13 120.3(2)
C11 C12 H12 119.8
C13 C12 H12 119.8
C12 C13 C14 120.8(2)
C12 C13 H13 119.6
C14 C13 H13 119.6
C13 C14 C9 117.7(2)
C13 C14 C16 119.8(2)
C9 C14 C16 122.4(2)
C10 C15 H15A 109.5
C10 C15 H15B 109.5
H15A C15 H15B 109.5
C10 C15 H15C 109.5
H15A C15 H15C 109.5
H15B C15 H15C 109.5
C14 C16 H16A 109.5
C14 C16 H16B 109.5
H16A C16 H16B 109.5
C14 C16 H16C 109.5
H16A C16 H16C 109.5
H16B C16 H16C 109.5
F1 C17 F3 109.1(4)
F1 C17 F2 109.4(3)
F3 C17 F2 109.1(3)
F1 C17 S1 111.1(3)
F3 C17 S1 108.9(3)
F2 C17 S1 109.2(3)
F6 C18 F4 108.9(3)
F6 C18 F5 108.8(4)
F4 C18 F5 109.2(4)
F6 C18 S2 111.0(3)
F4 C18 S2 109.1(3)
F5 C18 S2 109.8(2)
S1 O1 P1 124.60(11)
S2 O4 P2 122.95(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 N2 1.701(2)
P1 N1 1.704(2)
P1 O1 1.7503(18)
P1 P2 2.5557(10)
P2 N1 1.697(2)
P2 N2 1.6977(19)
P2 O4 1.7491(17)
S1 O3 1.398(3)
S1 O2 1.408(3)
S1 O1 1.5529(18)
S1 C17 1.807(4)
S2 O5 1.397(3)
S2 O6 1.411(2)
S2 O4 1.5508(18)
S2 C18 1.830(5)
N1 C1 1.443(3)
N2 C9 1.441(3)
C1 C2 1.400(4)
C1 C6 1.400(4)
C2 C3 1.393(4)
C2 C7 1.507(4)
C3 C4 1.386(5)
C3 H3 0.9500
C4 C5 1.370(5)
C4 H4 0.9500
C5 C6 1.396(4)
C5 H5 0.9500
C6 C8 1.506(4)
C7 H7A 0.9800
C7 H7B 0.9800
C7 H7C 0.9800
C8 H8A 0.9800
C8 H8B 0.9800
C8 H8C 0.9800
C9 C10 1.399(3)
C9 C14 1.402(3)
C10 C11 1.392(3)
C10 C15 1.510(3)
C11 C12 1.377(4)
C11 H11 0.9500
C12 C13 1.385(4)
C12 H12 0.9500
C13 C14 1.396(3)
C13 H13 0.9500
C14 C16 1.506(3)
C15 H15A 0.9800
C15 H15B 0.9800
C15 H15C 0.9800
C16 H16A 0.9800
C16 H16B 0.9800
C16 H16C 0.9800
C17 F1 1.298(5)
C17 F3 1.313(5)
C17 F2 1.323(4)
C18 F6 1.298(4)
C18 F4 1.319(4)
C18 F5 1.328(5)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 21120134
