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_7228261
_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         'C8 H3 O7 Tb, 4(H2 O)'
_chemical_formula_sum            'C8 H11 O11 Tb'
_chemical_formula_weight         442.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2017-05-01 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.121(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3720(10)
_cell_length_b                   6.5373(4)
_cell_length_c                   16.4809(12)
_cell_measurement_reflns_used    6994
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.577
_cell_measurement_theta_min      2.729
_cell_volume                     1316.11(17)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0874
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15766
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         28.961
_diffrn_reflns_theta_min         2.440
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.762
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.5543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1088 before and 0.0836 after correction.
The Ratio of minimum to maximum transmission is 0.7424.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.01
_refine_diff_density_max         8.267
_refine_diff_density_min         -10.674
_refine_diff_density_rms         0.554
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2673
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.1081
_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^)+294.2910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2569
_refine_ls_wR_factor_ref         0.2649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2184
_reflns_number_total             2673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00589j2.cif
_cod_data_source_block           Sion-1_H2O
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7228261
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.877
_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(O6) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C8(H8)
3.b Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'