Structural reorganization in a hydrogen-bonded organic framework
Castells-Gil, Javier; Padial, Natalia M.; Martí-Gastaldo, Carlos; New Journal of Chemistry 42 (2018) 16138–; doi:10.1039/C8NJ02738B

data_7057681
_publ_section_title
;
 Structural reorganization in a hydrogen-bonded organic framework
;
_journal_issue                   19
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16138
_journal_paper_doi               10.1039/C8NJ02738B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C16 H8 N2 O8, 2(H2 O), 2(C H6 N3)'
_chemical_formula_sum            'C18 H24 N8 O10'
_chemical_formula_weight         512.45
_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   mixed
_audit_creation_date             2018-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-09 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.738(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.8679(6)
_cell_length_b                   18.4531(7)
_cell_length_c                   7.0790(3)
_cell_measurement_reflns_used    6214
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.0580
_cell_measurement_theta_min      4.7500
_cell_volume                     2195.92(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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      150.0(10)
_diffrn_detector_area_resol_mean 5.2977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_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    -74.00 -14.00   1.00   10.00    --  -41.36  77.00 150.00   60
  2  \w    -50.00  13.00   1.00   10.00    --  -41.36  38.00  30.00   63
  3  \w   -121.00  -3.00   1.00   10.00    --  -41.36 -19.00  30.00  118
  4  \w    -72.00 -18.00   1.00   10.00    --  -41.36 125.00-150.00   54
  5  \w    -44.00  27.00   1.00   10.00    --  -41.36  38.00  90.00   71
  6  \w     64.00  90.00   1.00   10.00    --   41.36-129.00 -15.00   26
  7  \w     30.00  88.00   1.00   40.00    --  106.58 -30.00  90.00   58
  8  \w     31.00  89.00   1.00   40.00    --  106.58 -30.00 -30.00   58
  9  \w     30.00 125.00   1.00   40.00    --  106.58 -77.00 -90.00   95
 10  \w     30.00  74.00   1.00   40.00    --  106.58 -30.00 150.00   44
 11  \w     60.00 120.00   1.00   40.00    --  106.58-125.00  90.00   60
 12  \w     31.00  88.00   1.00   40.00    --  106.58 -30.00 -90.00   57
 13  \w     32.00  90.00   1.00   40.00    --  106.58 -30.00  30.00   58
 14  \w    116.00 143.00   1.00   40.00    --  106.58  45.00-180.00   27
 15  \w     37.00  64.00   1.00   40.00    --  106.58 -30.00 120.00   27
 16  \w     58.00 119.00   1.00   40.00    --  106.58-125.00 -90.00   61
 17  \w    101.00 128.00   1.00   40.00    --  106.58 125.00  30.00   27
 18  \w    153.00 178.00   1.00   40.00    --  106.58 125.00  30.00   25
 19  \w     25.00 156.00   1.00   40.00    --  106.58 -15.00-180.00  131
 20  \w     38.00 131.00   1.00   40.00    --  106.58 -77.00  90.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            12465
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        58.920
_diffrn_reflns_theta_max         58.920
_diffrn_reflns_theta_min         3.557
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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 light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         3114
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0922
_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^)+(0.1733P)^2^+9.5372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2853
_refine_ls_wR_factor_ref         0.2890
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2800
_reflns_number_total             3114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02738b2.cif
_cod_data_source_block           1576297
_cod_depositor_comments
'Adding full bibliography for 7057680--7057681.cif.'
_cod_database_code               7057681
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4(0.044) H8(0.041) H2(0.024) H4A(0.023) H6(0.025) H10(0.024)
 H12(0.021) H14(0.024) H1WA(0.053) H1WB(0.053) H1AA(0.033) H1AB(0.033)
 H2AA(0.043) H2AB(0.043) H3AA(0.036) H3AB(0.036) H2WA(0.056) H2WB(0.056)
 H1BA(0.035) H1BB(0.035) H2BA(0.044) H2BB(0.044) H3BA(0.036) H3BB(0.036)
 Fixed X: H4(1.014451) H8(0.503123) H2(0.859398) H4A(1.067754) H6(0.876926)
 H10(0.650593) H12(0.443081) H14(0.636544) H1WA(0.771331) H1WB(0.844498)
 H1AA(0.851217) H1AB(0.857232) H2AA(0.657675) H2AB(0.732297) H3AA(0.665067)
 H3AB(0.744956) H2WA(0.649117) H2WB(0.651769) H1BA(0.814885) H1BB(0.852187)
 H2BA(0.70082) H2BB(0.784324) H3BA(0.644035) H3BB(0.689536)
 Fixed Y: H4(0.446659) H8(-0.021073) H2(0.118874) H4A(0.212697) H6(0.337873)
 H10(0.308347) H12(0.212527) H14(0.090041) H1WA(-0.043966) H1WB(-0.012539)
 H1AA(0.00579) H1AB(0.025417) H2AA(0.037186) H2AB(0.014201) H3AA(0.06572)
 H3AB(0.061546) H2WA(-0.106822) H2WB(-0.085895) H1BA(-0.293524) H1BB(-0.224072)
 H2BA(-0.115127) H2BB(-0.118032) H3BA(-0.217651) H3BB(-0.289087)
 Fixed Z: H4(0.762889) H8(0.216734) H2(0.57852) H4A(0.768079) H6(0.611027)
 H10(0.416827) H12(0.225048) H14(0.379575) H1WA(0.458099) H1WB(0.433151)
 H1AA(1.067505) H1AB(0.86003) H2AA(1.073915) H2AB(1.195232) H3AA(0.761106)
 H3AB(0.675578) H2WA(0.40148) H2WB(0.590231) H1BA(-0.020067) H1BB(-0.088467)
 H2BA(-0.023293) H2BB(-0.090415) H3BA(0.08591) H3BB(0.091821)
;
_shelx_res_checksum              29057
_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
;