Proton Conduction in a Phosphonate-Based Metal-Organic Framework Mediated by Intrinsic "Free Diffusion inside a Sphere".
Pili, Simona; Argent, Stephen P.; Morris, Christopher G.; Rought, Peter; García-Sakai, Victoria; Silverwood, Ian P.; Easun, Timothy L.; Li, Ming; Warren, Mark R.; Murray, Claire A.; Tang, Chiu C.; Yang, Sihai; Schröder, Martin; Journal of the American Chemical Society 138 (2016) 6352–6355; doi:10.1021/jacs.6b02194

data_4130318
_publ_section_title
;
 Proton Conduction in a Phosphonate-Based Metal-Organic Framework Mediated
 by Intrinsic &quot;Free Diffusion inside a Sphere&quot;.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6352
_journal_page_last               6355
_journal_paper_doi               10.1021/jacs.6b02194
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
'C49.9 H35.71 Ni3 O27.95 P6 S0.95, 6(O0.32 S0.05)'
_chemical_formula_sum            'C54 H72 N0 Ni3 O30 P6 S3'
_chemical_formula_weight         1659.24
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.323(6)
_cell_length_b                   16.323(6)
_cell_length_c                   14.933(8)
_cell_measurement_reflns_used    10494
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      1.4
_cell_volume                     3446(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 0.0350
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
	Number of images: 188
	           Slice: -72.0000 - 116.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 120.0000
	             XTD: 59.4322
	          2theta: 30.1240
scan:
	Number of images: 140
	           Slice: -72.0000 - 68.0000
	     Image width: 1.0000
	        Exp time: 1.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -40.0000
	             Phi: 270.0000
	             XTD: 59.4322
	          2theta: 30.1240
;
_diffrn_measurement_device       'CrystalLogic Kappa (4 circle)'
_diffrn_measurement_device_type  'Kappa Rigaku Saturn724+'
_diffrn_measurement_method       'omega rotation'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.063067
_diffrn_orient_matrix_UB_12      -0.032033
_diffrn_orient_matrix_UB_13      0.000996
_diffrn_orient_matrix_UB_21      -0.059152
_diffrn_orient_matrix_UB_22      0.038119
_diffrn_orient_matrix_UB_23      -0.007248
_diffrn_orient_matrix_UB_31      0.003001
_diffrn_orient_matrix_UB_32      -0.007974
_diffrn_orient_matrix_UB_33      -0.066421
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'Synchrotron '
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1315
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20957
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         26.590
_diffrn_reflns_theta_min         1.396
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Scale-CrystalClear-SM Expert 2.0 r13 (Rigaku, 2011)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.675
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2734
_refine_ls_number_restraints     236
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0839
_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^)+(0.1690P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2414
_refine_ls_wR_factor_ref         0.2629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1462
_reflns_number_total             2734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b02194_si_003.cif
_cod_data_source_block           nisplb
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4130318
_nottingham_internal_coll_name   NISPLC
_nottingham_internal_coll_number 11972
_nottingham_internal_coll_client SP/SY/MS
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time 1.0000
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxsp5
_nottingham_internal_coll_date   19/02/2013
_nottingham_internal_coll_location DLS
_nottingham_internal_process_date 19/02/2013
_nottingham_internal_process_user pcxsp5
_nottingham_internal_solution_date 19/02/2013
_nottingham_internal_solution_user pcxsp5/pczsy
_nottingham_internal_refinement_date 11/01/2016
_nottingham_internal_refinement_user pcxsp5/pczsy/pczspa
_nottingham_internal_validation_date 26/01/2016
_nottingham_internal_validation_user AJB
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.903
_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
2. Restrained distances
 S2A_$1-O1A_$1
 1.68 with sigma of 0.005
 C3A_$2-C3A_$1
 2.81 with sigma of 0.01
 C3A_$2-O1A_$2
 2.83 with sigma of 0.01
 S2A_$1-C3A_$1 = S2A_$1-C3A_$2
 1.88 with sigma of 0.005
 S2B-O1B
 1.67 with sigma of 0.02
3. Restrained planarity
 C21A, C22A, C23A, C25A, C26A, C24A
 with sigma of 0.05
 C21A, C22B, C23B, C25B, C26B, C24A
 with sigma of 0.05
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C25B)=Sof(H25B)=Sof(C26B)=
 Sof(H26B)=1-FVAR(1)
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=
 Sof(H26A)=FVAR(1)
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=2*(1-FVAR(3))
 Sof(O1A)=Sof(S2A)=1-FVAR(2)
 Sof(Ni3)=0.33333*(1-FVAR(3))
 Sof(Ni2)=0.33333*FVAR(3)
 Fixed Sof: Ni1(0.16667)
 Fixed Uiso: O1B(0.08) S2B(0.08)
 Fixed X: O1A(0.42349)
 Fixed Y: O1A(0.768901)
 Fixed Z: O1A(0.75)
7.a Me refined with riding coordinates:
 C3A(H3AA,H3AB,H3AC)
7.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C22A(H22A), C23A(H23A), C25A(H25A), C26A(H26A), C22B(H22B),
 C23B(H23B), C25B(H25B), C26B(H26B)
;
_shelx_res_checksum              20443
_shelx_hkl_checksum              59701
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'