Role of entropic effects in controlling the polymorphism in formate ABX3 metal-organic frameworks
Gregor Kieslich; Shohei Kumagai; Keith T. Butler; Takuro Okamura; Christopher H. Hendon; Shijing Sun; Masahiro Yamashita; Aron Walsh; Anthony K. Cheetham; Chem.Commun. 51 (2015) 15538–; doi:10.1039/C5cc06190C

data_7117948
_publ_section_title
;
 Role of entropic effects in controlling the polymorphism in formate ABX3
 metal-organic frameworks
;
_journal_name_full               Chem.Commun.
_journal_page_first              15538
_journal_paper_doi               10.1039/C5cc06190C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C3 H3 O6 Zn, H5 N2'
_chemical_formula_sum            'C3 H8 N2 O6 Zn'
_chemical_formula_weight         233.48
_chemical_name_systematic        'Hydrazinium zinc formate'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   other
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-08-13 deposited with the CCDC.
2015-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.29731(6)
_cell_length_b                   7.94804(7)
_cell_length_c                   13.82240(12)
_cell_measurement_reflns_used    21150
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      36.9350
_cell_measurement_theta_min      2.9490
_cell_volume                     801.690(12)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0546400000
_diffrn_orient_matrix_UB_12      -0.0699273000
_diffrn_orient_matrix_UB_13      -0.0135835000
_diffrn_orient_matrix_UB_21      0.0206233000
_diffrn_orient_matrix_UB_22      0.0398123000
_diffrn_orient_matrix_UB_23      -0.0446172000
_diffrn_orient_matrix_UB_31      0.0777104000
_diffrn_orient_matrix_UB_32      0.0385656000
_diffrn_orient_matrix_UB_33      0.0214052000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47309
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.317
_diffrn_reflns_theta_min         2.947
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.060
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET) (compiled Aug 4 2014,14:34:23) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.934
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.6582
_exptl_crystal_size_mid          0.2766
_exptl_crystal_size_min          0.209
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 1602 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.002(3)
_refine_ls_extinction_coef       0.0204(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         3869
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0151
_refine_ls_R_factor_gt           0.0144
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+0.0842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0375
_reflns_Friedel_coverage         0.748
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                3790
_reflns_number_total             3869
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc06190c2.cif
_cod_data_source_block           Zn1O6C3N2H8
_cod_database_code               7117948
_chemical_oxdiff_formula         'Zn1 O6 C3 H8 N2'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All N(H,H) groups
2. Restrained distances
 H2B-N2
 0.89 with sigma of 0.001
 H2A-N2
 0.89 with sigma of 0.001
 H2B-H2A
 1.453 with sigma of 0.001
 H2B-N1
 1.916 with sigma of 0.001
 H2A-N1
 1.916 with sigma of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'