Supramolecular zwitterions based on a novel boronic acid‒squarate dianion synthon
Fornasari, Luca; d'Agostino, Simone; Braga, Dario; CrystEngComm 21 (2019) 3186–; doi:10.1039/C9CE00367C

data_7232605
_publ_section_title
;
 Supramolecular zwitterions based on a novel boronic acid--squarate
 dianion synthon
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              3186
_journal_paper_doi               10.1039/C9CE00367C
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C4 O4, 2(H2 O), 2(C5 H7 B N O2)'
_chemical_formula_sum            'C14 H18 B2 N2 O10'
_chemical_formula_weight         395.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-28 deposited with the CCDC.    2019-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.556(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   3.7455(3)
_cell_length_b                   10.5330(6)
_cell_length_c                   21.5313(12)
_cell_measurement_reflns_used    1268
_cell_measurement_temperature    250
_cell_measurement_theta_max      28.9530
_cell_measurement_theta_min      3.8000
_cell_volume                     846.75(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      250
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -57.00 -52.00   1.00   10.00    --  -17.60 134.00  14.00    5
  2  \w     28.00  33.00   1.00   10.00    --  -17.60  70.00  90.00    5
  3  \w     28.00  33.00   1.00   10.00    --   19.16 -70.00  90.00    5
  4  \w    -15.00  23.00   1.00   15.00    --  -17.75 -99.00  30.00   38
  5  \w     44.00  94.00   1.00   15.00    --   19.00-178.00 -30.00   50
  6  \w      2.00  83.00   1.00   15.00    --   19.00  38.00  90.00   81
  7  \w    -22.00  55.00   1.00   15.00    --   19.00 -99.00-180.00   77
  8  \w    -53.00  45.00   1.00   15.00    --   19.00 -38.00 -90.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0218117000
_diffrn_orient_matrix_UB_12      0.0644058000
_diffrn_orient_matrix_UB_13      -0.0084945000
_diffrn_orient_matrix_UB_21      0.1886492000
_diffrn_orient_matrix_UB_22      -0.0077171000
_diffrn_orient_matrix_UB_23      0.0032572000
_diffrn_orient_matrix_UB_31      -0.0021540000
_diffrn_orient_matrix_UB_32      -0.0179835000
_diffrn_orient_matrix_UB_33      -0.0317935000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            2893
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.001
_diffrn_reflns_theta_min         3.442
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.130
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       prism
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.229
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0571P)^2^+0.3930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                782
_reflns_number_total             884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00367c2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7232605--7232608.cif.'
_cod_database_code               7232605
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.938
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Free rotating group:
 O3(H3A)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C4(H4)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              11924
_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 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.810