Boric Acid Co-crystals in Guar Gelation
Perrin, Andrea; Goodwin, Melissa J.; Musa, Osama; Yufit, Dimitrii S.; Steed, Jonathan W.; CrystEngComm  (2017) –; doi:10.1039/C7CE01858D

data_7229587
_publ_section_title
;
 Boric Acid Co-crystals in Guar Gelation
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01858D
_journal_year                    2017
_chemical_formula_moiety         '2(B H3 O3), C12 H20 N2 O3'
_chemical_formula_sum            'C12 H26 B2 N2 O9'
_chemical_formula_weight         363.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-07-03
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_audit_update_record
;
2017-08-11 deposited with the CCDC.
2017-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                79.301(5)
_cell_angle_beta                 80.217(5)
_cell_angle_gamma                68.622(5)
_cell_formula_units_Z            2
_cell_length_a                   7.0629(4)
_cell_length_b                   7.9863(4)
_cell_length_c                   17.6846(9)
_cell_measurement_reflns_used    2884
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.6070
_cell_measurement_theta_min      2.7586
_cell_volume                     907.03(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.9964
_diffrn_measured_fraction_theta_max 0.9964
_diffrn_measurement_details
;
  1 omega  -50.00   44.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429   77.0000    0.0000 94

  2 omega  -49.00   -2.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -77.0000  150.0000 47

  3 omega  -89.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -77.0000 -120.0000 89

  4 omega  -37.00   -5.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -57.0000 -120.0000 32

  5 omega  -17.00  100.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679   19.0000 -180.0000 117

  6 omega    6.00   73.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -109.0000   98.0000 67

  7 omega  -99.00   -1.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429  -38.0000  -30.0000 98

  8 omega  -42.00  -10.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  -57.0000 -120.0000 32

  9 omega   56.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  179.0000  -60.0000 47
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0459460000
_diffrn_orient_matrix_UB_12      -0.0417415000
_diffrn_orient_matrix_UB_13      0.0332300000
_diffrn_orient_matrix_UB_21      -0.0730081000
_diffrn_orient_matrix_UB_22      -0.0027246000
_diffrn_orient_matrix_UB_23      -0.0223432000
_diffrn_orient_matrix_UB_31      0.0658532000
_diffrn_orient_matrix_UB_32      -0.0866909000
_diffrn_orient_matrix_UB_33      -0.0091497000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10266
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.76
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.3695
_exptl_crystal_size_min          0.1711
_refine_diff_density_max         0.212
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.1429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3067
_reflns_number_total             3945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce01858d2.cif
_cod_data_source_block           1x2B_ap91_1b
_cod_original_cell_volume        907.03(8)
_cod_database_code               7229587
_chemical_oxdiff_formula         C12H26N2O9B2
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H2A,H2B} of C2, {H3A,H3B} of C3, {H7A,H7B} of C7, {H6A,H6B} of C6, {H8A,
  H8B} of C8, {H5A,H5B} of C5, {H10A,H10B} of C10, {H12A,H12B} of C12, {H4A,
  H4B} of C4, {H11A,H11B} of C11
 At 1.5 times of:
  H9 of O9, H5 of O5, H4 of O4, H6 of O6, H7 of O7
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C8(H8A,H8B), C6(H6A,H6B), C7(H7A,H7B), C3(H3A,H3B), C2(H2A,H2B),
 C10(H10A,H10B), C12(H12A,H12B), C4(H4A,H4B), C11(H11A,H11B)
2.b Idealised tetrahedral OH refined as rotating group:
 O6(H6), O7(H7), O4(H4), O9(H9), O5(H5)
;