Crystalline structure of an ammonia borane‒polyethylene oxide cocrystal: a material investigated for its hydrogen storage potential
Ploszajski, Anna R.; Billing, Matthew; Cockcroft, Jeremy K.; Skipper, Neal T.; CrystEngComm 20 (2018) 4436–; doi:10.1039/C8CE00872H

data_7231073
_publ_section_title
;
 Crystalline structure of an ammonia borane--polyethylene oxide cocrystal:
 a material investigated for its hydrogen storage potential
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              4436
_journal_paper_doi               10.1039/C8CE00872H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C10 H20 O5, B H6 N'
_chemical_formula_sum            'C10 H26 B N O5'
_chemical_formula_weight         251.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-05-22 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.676(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4668(7)
_cell_length_b                   8.4576(8)
_cell_length_c                   20.568(2)
_cell_measurement_reflns_used    2024
_cell_measurement_temperature    295.
_cell_measurement_theta_max      50.3880
_cell_measurement_theta_min      5.6450
_cell_volume                     1472.7(2)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     48.00  74.00   1.00   10.00    --    0.00  77.00 -30.00   26
  2  \w     12.00  73.00   1.00   10.00    --    0.00  77.00  30.00   61
  3  \w     29.00 133.00   1.00   20.00    --   61.95  77.00 150.00  104
  4  \w    106.00 135.00   1.00   20.00    --   61.95  77.00 120.00   29
  5  \w     79.00 138.00   1.00   20.00    --   61.95  77.00  90.00   59
  6  \w     60.00 118.00   1.00   20.00    --   61.95  77.00  30.00   58
  7  \w     76.00 121.00   1.00   20.00    --   61.95  77.00 -90.00   45
  8  \w     82.00 137.00   1.00   20.00    --   61.95  76.00-124.81   55
  9  \w     67.00 115.00   1.00   20.00    --   61.95  75.00-151.76   48
 10  \w     30.00  63.00   1.00   20.00    --   61.95  75.00-151.76   33
 11  \w     29.00  54.00   1.00   20.00    --   61.95  77.00 -90.00   25
 12  \w     29.00  59.00   1.00   20.00    --   61.95  77.00 -60.00   30
 13  \w     29.00 136.00   1.00   20.00    --   61.95  77.00 -30.00  107
 14  \w     29.00  55.00   1.00   20.00    --   61.95  77.00  30.00   26
 15  \w     30.00 131.00   1.00   20.00    --   61.95  77.00  60.00  101
 16  \w     29.00  55.00   1.00   20.00    --   61.95  77.00  90.00   26
 17  \w     30.00  57.00   1.00   20.00    --   61.95  77.00 120.00   27
 18  \w     30.00  56.00   1.00   20.00    --   61.95  77.00   0.00   26
 19  \w     30.00  56.00   1.00   20.00    --   61.95  76.00-124.81   26
 20  \w    -32.00  44.00   1.00   10.00    --    0.00  77.00 -30.00   76
 21  \w    -31.00  45.00   1.00   10.00    --    0.00  77.00 120.00   76
 22  \w    -11.00  87.00   1.00   20.00    --   61.95 -57.00  30.00   98
 23  \w     33.00 118.00   1.00   20.00    --   61.95-125.00  30.00   85
 24  \w     -9.00  90.00   1.00   20.00    --   61.95 -57.00-150.00   99
 25  \w    -11.00  95.00   1.00   20.00    --   61.95 -77.00 150.00  106
;
_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      0.0456852000
_diffrn_orient_matrix_UB_12      0.0149777000
_diffrn_orient_matrix_UB_13      -0.0720061000
_diffrn_orient_matrix_UB_21      0.1404615000
_diffrn_orient_matrix_UB_22      0.1065770000
_diffrn_orient_matrix_UB_23      0.0194565000
_diffrn_orient_matrix_UB_31      0.1063460000
_diffrn_orient_matrix_UB_32      -0.1469277000
_diffrn_orient_matrix_UB_33      0.0068195000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10551
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        51.742
_diffrn_reflns_theta_max         51.742
_diffrn_reflns_theta_min         5.656
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.926
_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    1.133
_exptl_crystal_description       needle
_exptl_crystal_F_000             552
_exptl_crystal_recrystallization_method
'Direct reaction of components on glass microscope slide'
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.143
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         1618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1190
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0957P)^2^+0.3193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.2091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                920
_reflns_number_total             1618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00872h2.cif
_cod_data_source_block           exp_1065
_cod_depositor_comments
'Adding full bibliography for 7231072--7231073.cif.'
_cod_original_cell_volume        1472.8(2)
_cod_database_code               7231073
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         '(CH2CH2O)5 BH3NH3'
_chemical_oxdiff_usercomment     'RT study for PXRD comparison'
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.38
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All B(H,H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
2.b Idealised Me refined as rotating group:
 N1(H1C,H1D,H1E), B1(H1F,H1G,H1H)
;
_olex2_date_sample_data_collection 2017-06-12
_olex2_exptl_crystal_mounting_method '20um Hampton Research nylon loop'
_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 2.185
_oxdiff_exptl_absorpt_empirical_full_min 0.390