A Novel Ammonium Pentaborate – Poly(ethylene-glycol) Templated Polymer-Inclusion Compound
Ploszajski, Anna Rebecca; Billing, Matthew; Skipper, Neal; Cockcroft, Jeremy Karl; Chemical Communications  (2019) –; doi:10.1039/C9CC02720C

data_7123714
_publ_section_title
;
 A Novel Ammonium Pentaborate -- Poly(ethylene-glycol) Templated
 Polymer-Inclusion Compound
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02720C
_journal_year                    2019
_chemical_formula_moiety         'B5 H4 O10, H4 N'
_chemical_formula_sum            'B5 H8 N O10'
_chemical_formula_weight         236.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-18 deposited with the CCDC.    2019-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.234(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.2922(2)
_cell_length_b                   17.3394(5)
_cell_length_c                   16.3648(5)
_cell_measurement_reflns_used    4405
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.4110
_cell_measurement_theta_min      4.7290
_cell_volume                     2636.10(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -5.00  30.00   1.00   15.00    --  -42.62  38.00 -30.00   35
  2  \w    -67.00 -35.00   1.00   15.00    --  -42.62  38.00 -30.00   32
  3  \w    -96.00 -17.00   1.00   15.00    --  -42.62 125.00  30.00   79
  4  \w   -114.00 -28.00   1.00   15.00    --  -42.62 -57.00-180.00   86
  5  \w     59.00 132.00   1.00   60.00    --  106.36 -30.00  90.00   73
  6  \w     91.00 175.00   1.00   60.00    --  106.36  30.00 150.00   84
  7  \w     95.00 164.00   1.00   60.00    --  106.36 125.00 150.00   69
  8  \w    112.00 171.00   1.00   60.00    --  106.36 125.00 -90.00   59
  9  \w     32.00  99.00   1.00   60.00    --  106.36 -95.00 -90.00   67
 10  \w     35.00 109.00   1.00   60.00    --  106.36-125.00  30.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0923077000
_diffrn_orient_matrix_UB_12      0.0570977000
_diffrn_orient_matrix_UB_13      -0.0507321000
_diffrn_orient_matrix_UB_21      -0.0541325000
_diffrn_orient_matrix_UB_22      -0.0668410000
_diffrn_orient_matrix_UB_23      -0.0544848000
_diffrn_orient_matrix_UB_31      -0.1266314000
_diffrn_orient_matrix_UB_32      -0.0129852000
_diffrn_orient_matrix_UB_33      0.0576617000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10626
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.564
_diffrn_reflns_theta_min         3.714
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.190
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5140
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0705P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4018
_reflns_number_total             5140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02720c2.cif
_cod_data_source_block           exp_1071
_cod_original_cell_volume        2636.12(13)
_cod_database_code               7123714
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         '(NH4 B5O10H4)2 (C2H4O)x'
_chemical_oxdiff_usercomment     'Crystals from heated PEO.AB'
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.911
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H1A-H1B \\sim H1A-H1C \\sim H1A-H1D \\sim H1B-H1C \\sim H1B-H1D \\sim H1C-H1D
\\sim H2A-H2B \\sim H2A-H2C
 \\sim H2A-H2D \\sim H2B-H2C \\sim H2B-H2D \\sim H2C-H2D
 with sigma of 0.001
 N1-H1A \\sim N1-H1B \\sim N1-H1C \\sim N1-H1D \\sim N2-H2A \\sim N2-H2B \\sim
N2-H2C \\sim N2-H2D
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uiso(H1A) = Uiso(H1B) = Uiso(H1C) = Uiso(H1D) = Uiso(H2A) = Uiso(H2B) =
Uiso(H2C) = Uiso(H2D)
4.a Idealised tetrahedral OH refined as rotating group:
 O7A(H7A), O8A(H8A), O9A(H9A), O10A(H10A), O7B(H7B), O8B(H8B), O9B(H9B),
 O10B(H10B)
;
_shelx_res_checksum              76544
_shelx_fab_checksum              17997
_olex2_date_sample_data_collection 2017-06-26
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.826