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_7228260
_publ_section_title
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 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         'C11 H10 N O7 Tb'
_chemical_formula_sum            'C11 H10 N O7 Tb'
_chemical_formula_weight         427.12
_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
_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                90
_cell_angle_beta                 98.599(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.388(3)
_cell_length_b                   6.6366(12)
_cell_length_c                   15.567(2)
_cell_measurement_reflns_used    5339
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.375
_cell_measurement_theta_min      2.173
_cell_volume                     1367.6(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14568
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.539
_diffrn_reflns_theta_min         2.647
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.200
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1157 before and 0.0610 after correction. The Ratio of minimum to maximum transmission is 0.7857. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.910
_refine_diff_density_min         -1.001
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4070
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0047P)^2^+2.2406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3034
_reflns_number_total             4070
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce00589j2.cif
_cod_data_source_block           SION-1
_cod_database_code               7228260
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N1-C2B \\sim N1-C3B
 with sigma of 0.02
 N1-C2A \\sim N1-C3A
 with sigma of 0.02
3. Restrained planarity
 N1, C3A, C1A, C2A
 with sigma of 0.1
 N1, C1B, C2B, C3B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C3B) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C2B)
\\sim Ueq: with sigma of 0.0075 and sigma for terminal atoms of 0.015
Uanis(O1B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1A) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
5. Others
 Sof(C1A)=Sof(H1AA)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(C1B)=Sof(H1BA)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(H2BC)=Sof(C3B)=Sof(H3BA)=
 Sof(H3BB)=Sof(H3BC)=FVAR(1)
 Sof(O1B)=Sof(H1B)=Sof(H13)=1-FVAR(2)
 Sof(O1A)=Sof(H1A)=Sof(H14)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C1A(H1AA), C1B(H1BA), C4(H4), C13(H13), C14(H14)
6.b Idealised Me refined as rotating group:
 C2A(H2AA,H2AB,H2AC), C2B(H2BA,H2BB,H2BC), C3A(H3AA,H3AB,H3AC), C3B(H3BA,H3BB,
 H3BC)
6.c Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O1B(H1B)
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_olex2_submission_special_instructions 'No special instructions were received'