Ionothermal synthesis of crystalline metal phosphites using multifunctional protic ionic liquids
Li, Ting; Mao, Yumei; Qi, Yue; Zeng, Hongmei; Zou, Guohong; Lin, Zhien; CrystEngComm  (2020) –; doi:10.1039/D0CE01182G

data_7241145
_publ_section_title
;
 Ionothermal synthesis of crystalline metal phosphites using
 multifunctional protic ionic liquids
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01182G
_journal_year                    2020
_chemical_formula_moiety         'F2 Fe2 H6 O8 P2, C4 H7 N2'
_chemical_formula_sum            'C4 H13 F2 Fe2 N2 O8 P2'
_chemical_formula_weight         428.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-14 deposited with the CCDC.	2020-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.713(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.06676(18)
_cell_length_b                   18.5492(6)
_cell_length_c                   7.3779(3)
_cell_measurement_reflns_used    2271
_cell_measurement_temperature    294.05(10)
_cell_measurement_theta_max      72.2620
_cell_measurement_theta_min      4.7700
_cell_volume                     652.77(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega    1.00   75.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  -90.0000 74

  2 omega   20.00  104.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -60.0000 84

  3 omega   23.00   90.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000   60.0000 67

  4 omega   23.00   90.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000    0.0000 67

  5 omega   90.00  175.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  120.0000 85

  6 omega   39.00  109.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  150.0000 70

  7 omega   40.00   98.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 58

  8 omega   39.00  109.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 70

  9 omega   39.00  109.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 70

 10 omega   10.00   96.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  120.0000 86

 11 omega  -11.00   26.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.6671  -57.0000 -180.0000 37

 12 omega   38.00   85.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.6671   57.0000   30.0000 47

 13 omega   61.00   87.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 26

 14 omega   50.00   79.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 29

 15 omega  123.00  164.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000    0.0000 41

 16 omega  135.00  161.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  150.0000 26

 17 omega  -31.00   53.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.6671  -57.0000  120.0000 84

 18 omega   10.00  104.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.6671   77.0000   30.0000 94

 19 omega  -31.00   53.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.6671  -57.0000   60.0000 84

 20 omega  -32.00    6.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.6671  -38.0000 -120.0000 38

 21 omega   20.00  104.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.6671   57.0000 -150.0000 84

 22 omega   69.00   96.00   1.0000    1.4700
omega____ theta____ kappa____ phi______ frames
    -       36.6671   57.0000    0.0000 27

 23 omega   42.00   98.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 56

 24 omega   45.00   88.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 43

 25 omega   63.00   89.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 26

 26 omega  100.00  144.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -30.0000 44

 27 omega  147.00  178.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -30.0000 31

 28 omega   47.00   78.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 31

 29 omega   82.00  107.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -60.0000 25

 30 omega   80.00  142.00   1.0000    5.8900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   90.0000 62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.2535103000
_diffrn_orient_matrix_UB_12      0.0462875000
_diffrn_orient_matrix_UB_13      0.1154220000
_diffrn_orient_matrix_UB_21      0.1790684000
_diffrn_orient_matrix_UB_22      -0.0686624000
_diffrn_orient_matrix_UB_23      0.0611480000
_diffrn_orient_matrix_UB_31      0.0894035000
_diffrn_orient_matrix_UB_32      0.0063565000
_diffrn_orient_matrix_UB_33      -0.1792840000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4763
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         4.768
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.804
_exptl_absorpt_correction_T_max  0.216
_exptl_absorpt_correction_T_min  0.040
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.182
_exptl_crystal_description       prism
_exptl_crystal_F_000             430
_exptl_crystal_size_max          0.4847
_exptl_crystal_size_mid          0.1715
_exptl_crystal_size_min          0.1204
_refine_diff_density_max         0.548
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0809P)^2^+0.4602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1095
_reflns_number_total             1199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01182g2.cif
_cod_data_source_block           1_CCDC1
_cod_database_code               7241145
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C8 H26 F4 Fe4 N4 O16 P4'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups, All P(H) groups
2. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H3C(0.5)
3.a Riding coordinates:
 P1(H1)
3.b Rotating group:
 O4(H4A,H4B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1A), C1(H1B)
3.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'