Hydrogen Storage in the Expanded Pore Metal‒Organic Frameworks M2(dobpdc) (M = Mg, Mn, Fe, Co, Ni, Zn)
Gygi, David; Bloch, Eric D.; Mason, Jarad A.; Hudson, Matthew R.; Gonzalez, Miguel I.; Siegelman, Rebecca L.; Darwish, Tamim A.; Queen, Wendy L.; Brown, Craig M.; Long, Jeffrey R.; Chemistry of Materials 28 (2016) 1128–; doi:10.1021/acs.chemmater.5b04538

data_4003225
_publ_section_title
;
 Hydrogen Storage in the Expanded Pore Metal--Organic Frameworks
 M2(dobpdc) (M = Mg, Mn, Fe, Co, Ni, Zn)
;
_journal_issue                   4
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1128
_journal_paper_doi               10.1021/acs.chemmater.5b04538
_journal_volume                  28
_journal_year                    2016
_chemical_formula_moiety         '0.33(C72 H84 Co6 N6 O24)'
_chemical_formula_sum            'C24 H28 Co2 N2 O8'
_chemical_formula_weight         590.34
_chemical_name_common            Co2(dobpdc)(DEF)2
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-17
_audit_creation_method
;
Olex2 1.2
(compiled Jan 19 2015 12:28:14 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.7036(5)
_cell_length_b                   21.7036(5)
_cell_length_c                   6.8440(2)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.942
_cell_measurement_theta_min      2.700
_cell_volume                     2791.93(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX 2'
_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, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            26757
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        30.162
_diffrn_reflns_theta_max         30.162
_diffrn_reflns_theta_min         2.339
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.671
_exptl_absorpt_correction_T_max  0.9420
_exptl_absorpt_correction_T_min  0.7483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1370 before and 0.0777 after correction.
The Ratio of minimum to maximum transmission is 0.7944.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.431
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2857
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0910P)^2^+4.1405P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1558
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2610
_reflns_number_total             2857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm5b04538_si_002.cif
_cod_data_source_block           rls001s
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2791.93(15)
_cod_database_code               4003225
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.921
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(4) 0.49(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 O4, N1, C12, C10A, C11B, C11A, C10B, C8B, C9A, C9B, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C10A(0.5) H10A(0.5) H10B(0.5) C11B(0.5) H11A(0.5) H11B(0.5)
 H11C(0.5) C11A(0.5) H11D(0.5) H11E(0.5) H11F(0.5) C10B(0.5) H10C(0.5)
 H10D(0.5) C8B(0.5) H8BA(0.5) H8BB(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5)
 C9B(0.5) H9BA(0.5) H9BB(0.5) H9BC(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C10A(H10A,H10B), C10B(H10C,H10D), C8B(H8BA,H8BB), C8A(H8AA,H8AB)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C3(H3), C12(H12)
5.c Idealised Me refined as rotating group:
 C11B(H11A,H11B,H11C), C11A(H11D,H11E,H11F), C9A(H9AA,H9AB,H9AC), C9B(H9BA,
 H9BB,H9BC)
;
_shelx_res_checksum              46102
_shelx_hkl_checksum              13729
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'