Formation Pathways of Metal Organic Frameworks Proceeding Through Partial Dissolution of the Metastable Phase
Anderson, Samantha; Gladysiak, Andrzej; Boyd, Peter G.; Ireland, Christopher; Miéville, Pascal; tiana, davide; Vlaisavljevich, Bess; Schouwink, Pascal; van Beek, Wouter; Gagnon, Kevin J.; Smit, Berend; Stylianou, Kyriakos; CrystEngComm  (2017) –; doi:10.1039/C7CE00589J

data_7228259
_publ_section_title
;
 Formation Pathways of Metal Organic Frameworks Proceeding Through Partial
 Dissolution of the Metastable Phase
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00589J
_journal_year                    2017
_chemical_formula_moiety         'C12 H6 O13 Tb, 3(H2 O)'
_chemical_formula_sum            'C12 H12 O16 Tb'
_chemical_formula_weight         571.14
_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
_audit_creation_date             2017-04-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-05-01 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                113.409(10)
_cell_angle_beta                 101.145(9)
_cell_angle_gamma                105.464(8)
_cell_formula_units_Z            2
_cell_length_a                   9.5715(9)
_cell_length_b                   10.1208(10)
_cell_length_c                   11.6980(13)
_cell_measurement_reflns_used    1984
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.2520
_cell_measurement_theta_min      2.0440
_cell_volume                     943.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.810
_diffrn_measured_fraction_theta_max 0.793
_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    -95.00 140.00   1.00   12.00    --    0.00   0.00   0.00  235
  2  \w    -15.00 130.00   1.00   12.00    --    0.00  40.00   0.00  145
  3  \w    -80.00  60.00   1.00   12.00    --    0.00 -40.00   0.00  140
  4  \w    -90.00  65.00   1.00   12.00    --    0.00  65.00   0.00  155
;
_diffrn_measurement_device_type  'Oxford diffraction, KM 6, Onyx'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0595590000
_diffrn_orient_matrix_UB_12      -0.0761549000
_diffrn_orient_matrix_UB_13      -0.0340861000
_diffrn_orient_matrix_UB_21      0.0534674000
_diffrn_orient_matrix_UB_22      -0.0325671000
_diffrn_orient_matrix_UB_23      -0.0222671000
_diffrn_orient_matrix_UB_31      0.0195788000
_diffrn_orient_matrix_UB_32      -0.0089948000
_diffrn_orient_matrix_UB_33      0.0579297000
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7153
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0890
_diffrn_reflns_Laue_measured_fraction_full 0.810
_diffrn_reflns_Laue_measured_fraction_max 0.793
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6544
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        25.416
_diffrn_reflns_theta_max         25.661
_diffrn_reflns_theta_min         2.029
_diffrn_source
;
ESRF, Swiss-Norwegian Beamline BM01
;
_exptl_absorpt_coefficient_mu    3.885
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37235
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            beige
_exptl_crystal_density_diffrn    2.011
_exptl_crystal_description       plate
_exptl_crystal_F_000             554
_exptl_crystal_size_max          0.565
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.820
_refine_diff_density_min         -4.956
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         2780
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1547P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1941
_refine_ls_wR_factor_ref         0.2209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2142
_reflns_number_total             2780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00589j2.cif
_cod_data_source_block           Sion-2_H2O
_cod_original_cell_volume        943.19(18)
_cod_database_code               7228259
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 79.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.66
_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. Uiso/Uaniso restraints and constraints
Uanis(C5) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C12)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4A), C7(H7), C12(H12)
3.b Tetrahedral OH refined with riding coordinates:
 O4(H4)
3.c Idealised tetrahedral OH refined as rotating group:
 O6(H6), O9(H9)
;
_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 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.609