Enhancement of CO2 Adsorption and Catalytic Properties by Fe-Doping of [Ga2(OH)2(L)] (H4L = Biphenyl-3,3',5,5'-tetracarboxylic Acid), MFM-300(Ga2).
Krap, Cristina P.; Newby, Ruth; Dhakshinamoorthy, Amarajothi; García, Hermenegildo; Cebula, Izabela; Easun, Timothy L.; Savage, Mathew; Eyley, Jennifer E.; Gao, Shan; Blake, Alexander J.; Lewis, William; Beton, Peter H.; Warren, Mark R.; Allan, David R.; Frogley, Mark D.; Tang, Chiu C.; Cinque, Gianfelice; Yang, Sihai; Schröder, Martin; Inorganic chemistry 55 (2016) 1076–1088; doi:10.1021/acs.inorgchem.5b02108

data_4344747
_publ_section_title
;
 Enhancement of CO2 Adsorption and Catalytic Properties by Fe-Doping of
 [Ga2(OH)2(L)] (H4L = Biphenyl-3,3',5,5'-tetracarboxylic Acid),
 MFM-300(Ga2).
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1076
_journal_page_last               1088
_journal_paper_doi               10.1021/acs.inorgchem.5b02108
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         '0.25(C64 H32 Fe0.4 Ga7.6 O40), 2.07(C O2)'
_chemical_formula_sum            'C18.06 H8 Fe0.1 Ga1.9 O14.12'
_chemical_formula_weight         588.94
_chemical_name_common            'MFM-300 (Ga1.9Fe0.1) 2.07CO2'
_space_group_crystal_system      tetragonal
_space_group_IT_number           98
_space_group_name_Hall           'I 4bw 2bw'
_space_group_name_H-M_alt        'I 41 2 2'
_symmetry_space_group_name_Hall  'I 4bw 2bw'
_symmetry_space_group_name_H-M   'I 41 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.924(8)
_cell_length_b                   14.924(8)
_cell_length_c                   11.929(9)
_cell_measurement_reflns_used    2800
_cell_measurement_temperature    195(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      2.1
_cell_volume                     2657(3)
_computing_cell_refinement       'Rigaku CrystalClear'
_computing_data_collection       'Rigaku CrystalClear'
_computing_data_reduction        'Rigaku CrystalClear'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      195.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12202
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.591
_diffrn_reflns_theta_min         2.118
_diffrn_source                   'Diamond beamline I19'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.034
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998). Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1163
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.60(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1526
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+1.2079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.710
_reflns_friedel_fraction_full    0.998
_reflns_friedel_fraction_max     0.998
_reflns_number_gt                1394
_reflns_number_total             1526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02108_si_002.cif
_cod_data_source_block           MFM-300_Ga1.9Fe0.1_2.07CO2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        2657(4)
_cod_original_formula_sum        'C18.06 H8 Fe0.10 Ga1.90 O14.12'
_cod_database_code               4344747
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.913
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.40(3) 0.60(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
3. Shared sites
{Ga1, Fe1}
4. Restrained distances
 C1S-O1S = C1S-O2S
 1.2 with sigma of 0.01
 C2S-O3S = C2S-O4S
 1.2 with sigma of 0.005
 O3S-O4S
 2.4 with sigma of 0.01
 C1S-O1S \\sim C1S-O2S
 with sigma of 0.01
 C2S-O3S \\sim C2S-O4S
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(Ga1) = Uanis(Fe1)
6. Others
 Sof(C1S)=Sof(O1S)=Sof(O2S)=0.5*FVAR(2)
 Sof(C2S)=Sof(O3S)=Sof(O4S)=0.5*FVAR(3)
 Uiso(C1S)=Uiso(O1S)=Uiso(O2S)=Uiso(C2S)=Uiso(O3S)=Uiso(O4S)=FVAR(3)
 Fixed Sof: Ga1(0.475) Fe1(0.025)
7.a Riding coordinates:
 O2(H2)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C5(H5)
;
_shelx_res_checksum              37428
_shelx_hkl_checksum              13486
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'