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_7229591
_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         'C6 H7 B O3'
_chemical_formula_sum            'C6 H7 B O3'
_chemical_formula_weight         137.93
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_audit_update_record
;
2017-08-11 deposited with the CCDC.
2017-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.695(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.3765(4)
_cell_length_b                   5.04525(19)
_cell_length_c                   17.3563(7)
_cell_measurement_reflns_used    3477
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.6500
_cell_measurement_theta_min      1.8248
_cell_volume                     1258.81(8)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -27.00   42.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  -57.0000   30.0000 69

  2 omega   43.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -178.0000   60.0000 60

  3 omega   12.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000  150.0000 57

  4 omega   37.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679 -100.0000  -90.0000 32

  5 omega   -2.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679   77.0000   60.0000 27

  6 omega    1.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679   38.0000  -60.0000 77

  7 omega  -46.00   71.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679  -19.0000   90.0000 117

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

  9 omega -102.00  -63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3429 -178.0000  150.0000 39

 10 omega    7.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679   57.0000  -30.0000 89

 11 omega   -3.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9679   77.0000  150.0000 100
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0187688000
_diffrn_orient_matrix_UB_12      -0.1069538000
_diffrn_orient_matrix_UB_13      0.0216623000
_diffrn_orient_matrix_UB_21      -0.0229261000
_diffrn_orient_matrix_UB_22      -0.0912438000
_diffrn_orient_matrix_UB_23      -0.0248938000
_diffrn_orient_matrix_UB_31      0.0394272000
_diffrn_orient_matrix_UB_32      -0.0020303000
_diffrn_orient_matrix_UB_33      -0.0241371000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15899
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         2.35
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.969
_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    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             576.000
_exptl_crystal_recrystallization_method
'The material was recrystallised from methanol by slow evaporation'
_exptl_crystal_size_max          0.4094
_exptl_crystal_size_mid          0.1855
_exptl_crystal_size_min          0.1143
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         2475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0516P)^2^+1.0331P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                2036
_reflns_number_total             2475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce01858d2.cif
_cod_data_source_block           4_ap68_13a
_cod_database_code               7229591
_chemical_oxdiff_formula         C6H7BO3
_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:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C2(H2), C3(H3A), C5(H5), C11(H11), C12(H12), C6(H6)
2.b Idealised tetrahedral OH refined as rotating group:
 O5(H5A), O6(H6A), O1(H1), O2(H2A)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems 700 Series'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perflourotether oil'
_olex2_submission_special_instructions 'No special instructions were received'