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_7229588
_publ_section_title
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 Boric Acid Co-crystals in Guar Gelation
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01858D
_journal_year                    2017
_chemical_formula_moiety         'C6 H8 B2 O4, C12 H20 N2 O3'
_chemical_formula_sum            'C18 H28 B2 N2 O7'
_chemical_formula_weight         406.04
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-09
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
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2017-08-11 deposited with the CCDC.
2017-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                112.5470(10)
_cell_angle_beta                 111.5550(10)
_cell_angle_gamma                94.5390(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0731(4)
_cell_length_b                   10.2343(4)
_cell_length_c                   12.1312(5)
_cell_measurement_reflns_used    6631
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      31.01
_cell_measurement_theta_min      2.23
_cell_volume                     1038.42(7)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'SMART 6K'
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18453
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.02
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.9606
_exptl_absorpt_correction_T_min  0.7497
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0651 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.7804.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.1400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                4790
_reflns_number_total             6065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce01858d2.cif
_cod_data_source_block           1xC6_15srv191
_cod_database_code               7229588
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Fixed Sof: H20C(0.5) H20D(0.5) H20A(0.5) H20B(0.5) C21A(0.5) H21A(0.5)
 H21B(0.5) C21B(0.5) H21C(0.5) H21D(0.5) H22C(0.5) H22D(0.5) H22A(0.5) H22B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C20(H20C,H20D), C20(H20A,
 H20B), C21A(H21A,H21B), C21B(H21C,H21D), C22(H22C,H22D), C22(H22A,H22B)
;