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_7241144
_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
'0.25(C24 H36 N4 O60 P20 Zn16), 0.25(H4 O2), 2(C6 H8 N)'
_chemical_formula_sum            'C18 H29 N3 O15.5 P5 Zn4'
_chemical_formula_weight         951.77
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-01
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5880(5)
_cell_length_b                   10.6964(3)
_cell_length_c                   21.1110(9)
_cell_measurement_reflns_used    3545
_cell_measurement_temperature    296.31(10)
_cell_measurement_theta_max      71.6650
_cell_measurement_theta_min      4.2300
_cell_volume                     3294.1(2)
_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      296.31(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -31.00   63.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000   90.0000 94

  2 omega  -35.00   66.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -19.0000   30.0000 101

  3 omega    1.00   75.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000 -120.0000 74

  4 omega   20.00  104.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -150.0000 84

  5 omega    5.00   31.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000    0.0000 26

  6 omega   44.00   95.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 51

  7 omega   52.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 39

  8 omega   43.00  116.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 73

  9 omega   52.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 39

 10 omega   40.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 51

 11 omega   76.00  106.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -150.0000 30
;
_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      -0.0829194000
_diffrn_orient_matrix_UB_12      -0.0496179000
_diffrn_orient_matrix_UB_13      -0.0375369000
_diffrn_orient_matrix_UB_21      -0.0590535000
_diffrn_orient_matrix_UB_22      0.0062102000
_diffrn_orient_matrix_UB_23      0.0604236000
_diffrn_orient_matrix_UB_31      -0.0277587000
_diffrn_orient_matrix_UB_32      0.1350660000
_diffrn_orient_matrix_UB_33      -0.0165631000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            8722
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         5.127
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.245
_exptl_absorpt_correction_T_max  0.549
_exptl_absorpt_correction_T_min  0.290
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.3204
_exptl_crystal_size_mid          0.1597
_exptl_crystal_size_min          0.1387
_refine_diff_density_max         1.398
_refine_diff_density_min         -2.135
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0894
_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/[\s^2^(Fo^2^)+(0.1826P)^2^+14.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2687
_refine_ls_wR_factor_ref         0.2789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2620
_reflns_number_total             3011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01182g2.cif
_cod_data_source_block           1
_cod_original_formula_sum        'C18 H29 N3 O15.50 P5 Zn4'
_cod_database_code               7241144
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C72  H104  N12  O62  P20  Zn16  '
_reflns_odcompleteness_completeness 99.16
_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: OW1(0.25) HW1A(0.25) HW1B(0.25) H6A(0.5) H6B(0.5) H6C(0.5)
3.a Riding coordinates:
 P3(H3), OW1(HW1A,HW1B), C6(H6A,H6B,H6C)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2A), C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              70747
_olex2_submission_special_instructions 'No special instructions were received'