#------------------------------------------------------------------------------
#$Date: 2019-11-23 17:43:03 +0100 (Sat 23 de Nov de 2019) $
#$Revision: 234486 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/50/7125070.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_7125070
loop_
_publ_author_name
'Jost, Maximilian'
'Finger, Lars H.'
'Sundermeyer, Jörg'
'von Hänisch, Carsten'
_publ_section_title
;
 Simple access to ionic liquids and organic salts containing the
 phosphaethynolate (PCO(-)) and Zintl (Sb11(3-)) anions.
;
_journal_issue                   78
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11646
_journal_page_last               11648
_journal_paper_doi               10.1039/c6cc06620h
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C4 H12 P, C O P'
_chemical_formula_sum            'C5 H12 O P2'
_chemical_formula_weight         150.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-27 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.159(5)
_cell_length_b                   7.4484(19)
_cell_length_c                   6.3101(15)
_cell_measurement_reflns_used    468
_cell_measurement_temperature    115.05
_cell_measurement_theta_max      24.797
_cell_measurement_theta_min      3.418
_cell_volume                     853.5(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      115.05
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2200
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.306
_diffrn_reflns_theta_min         2.243
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0989 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.7230.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       needle
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         841
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0460
_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)+(0.0230P)²+0.8167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0900
_reflns_Friedel_coverage         0.000
_reflns_number_gt                573
_reflns_number_total             841
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6cc06620h2.cif
_cod_data_source_block           compound3
_cod_database_code               7125070
_shelxl_version_number           2014-3
_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_max   0.991
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
4.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C)
;
_shelx_res_file
;
TITL Mj54_0ma in Pnma
CELL 0.71073 18.1592 7.4484 6.3101 90 90 90
ZERR 4 0.005 0.0019 0.0015 0 0 0
LATT 1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,-Z
SYMM 0.5+X,0.5-Y,0.5-Z
SFAC C H O P
UNIT 20 48 4 8
RIGU

L.S. 20
PLAN  20
SIZE 0.022 0.036 0.258
TEMP -158.1
BOND
LIST 6
fmap 2
acta
MERG 2
REM <olex2.extras>
REM <HklSrc "%.\\Mj54_0ma_a.hkl">
REM </olex2.extras>

WGHT    0.023000    0.816700
FVAR       0.71566
P1    4    0.373926    0.750000    0.495010    10.50000    0.01745    0.01860 =
         0.01928    0.00000    0.00086    0.00000
C2    1    0.456105    0.750000    0.649194    10.50000    0.02204    0.02933 =
         0.02952    0.00000   -0.00208    0.00000
PART -1
AFIX 137
H2A   2    0.461099    0.634395    0.721942    10.50000   -1.50000
H2B   2    0.453785    0.846755    0.754226    10.50000   -1.50000
H2C   2    0.498640    0.768850    0.556232    10.50000   -1.50000
AFIX   0
PART 0
C3    1    0.297769    0.750000    0.673043    10.50000    0.02281    0.02852 =
         0.02702    0.00000    0.00340    0.00000
PART -1
AFIX 137
H3A   2    0.302093    0.851919    0.770470    10.50000   -1.50000
H3B   2    0.297489    0.637802    0.754159    10.50000   -1.50000
H3C   2    0.251836    0.760278    0.592423    10.50000   -1.50000
AFIX   0
PART 0
C1    1    0.372356    0.556340    0.330038    11.00000    0.02675    0.02221 =
         0.02855   -0.00192    0.00117    0.00138
AFIX 137
H1A   2    0.415381    0.557487    0.236296    11.00000   -1.50000
H1B   2    0.327301    0.556684    0.244551    11.00000   -1.50000
H1C   2    0.373522    0.448173    0.418393    11.00000   -1.50000
AFIX   0
O1    3    0.716166    0.750000    0.331987    10.50000    0.02817    0.05665 =
         0.04476    0.00000    0.00405    0.00000
C4    1    0.656736    0.750000    0.244290    10.50000    0.02970    0.02634 =
         0.02422    0.00000    0.01121    0.00000
P2    4    0.579304    0.750000    0.130534    10.50000    0.03664    0.03257 =
         0.02513    0.00000    0.00047    0.00000
HKLF 4

REM  Mj54_0ma in Pnma
REM R1 =  0.0460 for     573 Fo > 4sig(Fo)  and  0.0857 for all     841 data
REM     49 parameters refined using     27 restraints

END

WGHT      0.0230      0.8167

REM Highest difference peak  0.440,  deepest hole -0.334,  1-sigma level  0.070
Q1    1   0.5784  0.7500  0.2775  10.50000  0.05    0.44
Q2    1   0.5779  0.7500 -0.0409  10.50000  0.05    0.31
Q3    1   0.2876  0.7500  0.9178  10.50000  0.05    0.26
Q4    1   0.4600  0.7500  0.1139  10.50000  0.05    0.25
Q5    1   0.3774  0.6941  0.3275  11.00000  0.05    0.24
Q6    1   0.6720  0.9194  0.1253  11.00000  0.05    0.24
Q7    1   0.6092  0.9012  0.1864  11.00000  0.05    0.24
Q8    1   0.4455  0.7500  0.5193  10.50000  0.05    0.23
Q9    1   0.3946  0.6213  0.4615  11.00000  0.05    0.22
Q10   1   0.7322  0.7500  0.3675  10.50000  0.05    0.22
Q11   1   0.3435  0.6050  0.4358  11.00000  0.05    0.22
Q12   1   0.5135  0.7500  0.4779  10.50000  0.05    0.22
Q13   1   0.6426  0.7500 -0.1112  10.50000  0.05    0.22
Q14   1   0.6760  0.7500  0.3496  10.50000  0.05    0.21
Q15   1   0.3002  0.7500  0.5008  10.50000  0.05    0.21
Q16   1   0.7086  0.8110  0.2269  11.00000  0.05    0.19
Q17   1   0.3564  0.5060  0.5605  11.00000  0.05    0.19
Q18   1   0.4262  0.6137  0.0225  11.00000  0.05    0.19
Q19   1   0.5031  0.7500  0.6564  10.50000  0.05    0.19
Q20   1   0.3974  0.4555  0.3389  11.00000  0.05    0.19
;
_shelx_res_checksum              45979
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.37393(6) 0.7500 0.4950(2) 0.0184(3) Uani 1 2 d S TU P . .
C2 C 0.4561(2) 0.7500 0.6492(7) 0.0270(11) Uani 1 2 d S TU P . .
H2A H 0.4611 0.6344 0.7219 0.040 Uiso 0.5 1 calc GR . . A -1
H2B H 0.4538 0.8468 0.7542 0.040 Uiso 0.5 1 calc GR . . A -1
H2C H 0.4986 0.7689 0.5562 0.040 Uiso 0.5 1 calc GR . . A -1
C3 C 0.2978(2) 0.7500 0.6730(7) 0.0261(12) Uani 1 2 d S TU P . .
H3A H 0.3021 0.8519 0.7705 0.039 Uiso 0.5 1 calc GR . . B -1
H3B H 0.2975 0.6378 0.7542 0.039 Uiso 0.5 1 calc GR . . B -1
H3C H 0.2518 0.7603 0.5924 0.039 Uiso 0.5 1 calc GR . . B -1
C1 C 0.37236(16) 0.5563(4) 0.3300(5) 0.0258(7) Uani 1 1 d . U . . .
H1A H 0.4154 0.5575 0.2363 0.039 Uiso 1 1 calc GR . . . .
H1B H 0.3273 0.5567 0.2446 0.039 Uiso 1 1 calc GR . . . .
H1C H 0.3735 0.4482 0.4184 0.039 Uiso 1 1 calc GR . . . .
O1 O 0.71617(17) 0.7500 0.3320(5) 0.0432(10) Uani 1 2 d S TU P . .
C4 C 0.6567(3) 0.7500 0.2443(7) 0.0268(11) Uani 1 2 d S TU P . .
P2 P 0.57930(7) 0.7500 0.1305(2) 0.0314(4) Uani 1 2 d S TU P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0174(6) 0.0186(6) 0.0193(6) 0.000 0.0009(5) 0.000
C2 0.022(2) 0.029(3) 0.030(3) 0.000 -0.002(2) 0.000
C3 0.023(2) 0.029(3) 0.027(3) 0.000 0.003(2) 0.000
C1 0.0268(16) 0.0222(16) 0.0286(17) -0.0019(16) 0.0012(15) 0.0014(16)
O1 0.0282(19) 0.057(3) 0.045(2) 0.000 0.0041(17) 0.000
C4 0.030(2) 0.026(3) 0.024(2) 0.000 0.011(2) 0.000
P2 0.0366(8) 0.0326(8) 0.0251(7) 0.000 0.0005(6) 0.000
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'
O O 0.0106 0.0060 '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'
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
C2 P1 C3 107.8(2) .
C1 P1 C2 109.45(13) .
C1 P1 C2 109.45(13) 7_575
C1 P1 C3 110.88(13) 7_575
C1 P1 C3 110.88(13) .
C1 P1 C1 108.3(2) 7_575
O1 C4 P2 179.9(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 C2 1.781(4) .
P1 C3 1.782(4) .
P1 C1 1.779(3) .
P1 C1 1.779(3) 7_575
O1 C4 1.213(5) .
C4 P2 1.579(5) .
