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_4344748
_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         '0.5(C96 H60 Fe12 O72)'
_chemical_formula_sum            'C48 H36 Fe6 O36'
_chemical_formula_weight         1523.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-07
_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                90
_cell_formula_units_Z            2
_cell_length_a                   10.5869(2)
_cell_length_b                   19.5108(4)
_cell_length_c                   11.8159(2)
_cell_measurement_reflns_used    4900
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.6900
_cell_measurement_theta_min      2.1230
_cell_volume                     2440.68(8)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48)'
_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_temperature      120(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.909
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_laue_measured_fraction_full 0.970
_diffrn_reflns_laue_measured_fraction_max 0.909
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11120
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         31.773
_diffrn_reflns_theta_min         2.121
_diffrn_source                   'Diamond beamline I19'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.716
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.284
_refine_diff_density_min         -2.032
_refine_diff_density_rms         0.257
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(10)
_refine_ls_extinction_coef       0.034(5)
_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   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         5874
_refine_ls_number_restraints     2325
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0964
_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^)+(0.0758P)^2^+37.6333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2384
_refine_ls_wR_factor_ref         0.2456
_reflns_Friedel_coverage         0.923
_reflns_friedel_fraction_full    0.973
_reflns_friedel_fraction_max     0.912
_reflns_number_gt                5775
_reflns_number_total             5874
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02108_si_002.cif
_cod_data_source_block           MFM-310_Fe
_cod_original_cell_volume        2440.69(8)
_cod_database_code               4344748
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(10) 0.46(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 C9-C6 \\sim C25-C22 \\sim C41-C38
 with sigma of 0.02
 C46-C41 \\sim C30-C25 \\sim C9-C10 \\sim C9-C14 \\sim C26-C25 \\sim C42-C41
\\sim C38-C37 \\sim C22-C21 ~
 C6-C5 \\sim C7-C6 \\sim C39-C38 \\sim C23-C22
 with sigma of 0.02
 C7-C2 \\sim C23-C18 \\sim C39-C34 \\sim C5-C4 \\sim C21-C20 \\sim C37-C36
\\sim C30-C29 \\sim C46-C45 ~
 C11-C10 \\sim C43-C42 \\sim C14-C13 \\sim C27-C26
 with sigma of 0.02
 C4-C3 \\sim C20-C19 \\sim C36-C35 \\sim C3-C2 \\sim C19-C18 \\sim C35-C34
\\sim C12-C11 \\sim C29-C28 ~
 C45-C44 \\sim C44-C43 \\sim C28-C27 \\sim C13-C12
 with sigma of 0.02
 O4-C4 \\sim C4-O3 \\sim O12-C20 \\sim C20-O11 \\sim O20-C36 \\sim C36-O19
\\sim O2-C2 \\sim C2-O1 \\sim O9-
 C18 \\sim C18-O10 \\sim O18-C34 \\sim C34-O17 \\sim O8-C13 \\sim C13-O7 \\sim
O6-C11 \\sim C11-O5 \\sim O15-
 C27 \\sim C27-O16 \\sim O14-C29 \\sim C29-O13 \\sim O22-C45 \\sim C45-O21
\\sim O23-C43 \\sim C43-O24
 with sigma of 0.02
 C8-C4 \\sim C24-C20 \\sim C40-C36 \\sim C2-C1 \\sim C18-C17 \\sim C34-C33
\\sim C16-C13 \\sim C32-C27 ~
 C48-C43 \\sim C15-C11 \\sim C31-C29 \\sim C47-C45
 with sigma of 0.02
 C5-C8 \\sim C8-C3 \\sim C7-C1 \\sim C1-C3 \\sim C14-C16 \\sim C16-C12 \\sim
C10-C15 \\sim C15-C12 \\sim C23-
 C17 \\sim C17-C19 \\sim C19-C24 \\sim C24-C21 \\sim C30-C31 \\sim C31-C28
\\sim C28-C32 \\sim C32-C26 ~
 C46-C47 \\sim C47-C44 \\sim C44-C48 \\sim C48-C42 \\sim C37-C40 \\sim C40-C35
\\sim C35-C33 \\sim C33-C39
 with sigma of 0.02
 O7-C16 \\sim O8-C16 \\sim O15-C32 \\sim O16-C32 \\sim O24-C48 \\sim O23-C48
\\sim O5-C15 \\sim O6-C15 ~
 O13-C31 \\sim O21-C47 \\sim O22-C47 \\sim O14-C31 \\sim O12-C24 \\sim O4-C8
\\sim O20-C40 \\sim O3-C8 ~
 O11-C24 \\sim O19-C40 \\sim O2-C1 \\sim O10-C17 \\sim O18-C33 \\sim O9-C17
\\sim O1-C1 \\sim O17-C33
 with sigma of 0.02
4. Restrained planarity
 C9, C10, C11, C12, C13, C14, C6, C3, C16, C15
 with sigma of 0.1
 C2, C3, C4, C5, C6, C7, C1, C8, C9, C12
 with sigma of 0.1
 C25, C26, C27, C28, C29, C30, C31, C22, C19, C32
 with sigma of 0.1
 C18, C19, C20, C21, C22, C23, C17, C24, C25, C28
 with sigma of 0.1
 C34, C35, C36, C37, C38, C39, C33, C40, C41, C44
 with sigma of 0.1
 O5, O6, C15, C11, C14
 with sigma of 0.1
 O7, O8, C13, C16, C10
 with sigma of 0.1
 O3, O4, C4, C8, C7
 with sigma of 0.1
 O1, O2, C1, C2, C5
 with sigma of 0.1
 O11, O12, C20, C24, C23
 with sigma of 0.1
 O9, O10, C17, C18, C21
 with sigma of 0.1
 C29, O13, O14, C31, C26
 with sigma of 0.1
 C30, O15, O16, C32, C27
 with sigma of 0.1
 O21, O22, C45, C47, C42
 with sigma of 0.1
 O17, O18, C33, C34, C37
 with sigma of 0.1
 C36, O20, C40, O19, C39
 with sigma of 0.1
 O3, C4, C7, C8, C2, C3, O4, C5, C9, C6, C1
 with sigma of 0.1
 C41, C42, C44, C45, C46, C47, C48, C35, C38, C43
 with sigma of 0.1
 O23, O24, C48, C43, C46
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.0025 and sigma
for terminal atoms of 0.005
6. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Others
 Fixed Sof: Fe2(0.5) Fe3(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) O5(0.5) O6(0.5)
 O7(0.5) O8(0.5) O9(0.5) O10(0.5) O11(0.5) O12(0.5) O13(0.5) O14(0.5) O15(0.5)
 O16(0.5) O17(0.5) O18(0.5) O19(0.5) O20(0.5) O21(0.5) O22(0.5) O23(0.5)
 O24(0.5) O28(0.5) H28A(0.5) H28B(0.5) H32A(0.5) H32B(0.5) C1(0.5) C2(0.5)
 C3(0.5) H3(0.5) C4(0.5) C5(0.5) H5(0.5) C6(0.5) C7(0.5) H7(0.5) C8(0.5)
 C9(0.5) C10(0.5) H10(0.5) C11(0.5) C12(0.5) H12(0.5) C13(0.5) C14(0.5)
 H14(0.5) C15(0.5) C16(0.5) C17(0.5) C18(0.5) C19(0.5) H19(0.5) C20(0.5)
 C21(0.5) H21(0.5) C22(0.5) C23(0.5) H23(0.5) C24(0.5) C25(0.5) C26(0.5)
 H26(0.5) C27(0.5) C28(0.5) H28(0.5) C29(0.5) C30(0.5) H30(0.5) C31(0.5)
 C32(0.5) C33(0.5) C34(0.5) C35(0.5) H35(0.5) C36(0.5) C37(0.5) H37(0.5)
 C38(0.5) C39(0.5) H39(0.5) C40(0.5) C41(0.5) C42(0.5) H42(0.5) C43(0.5)
 C44(0.5) H44(0.5) C45(0.5) C46(0.5) H46(0.5) C47(0.5) C48(0.5)
8.a Rotating group:
 O28(H28A,H28B), O30(H30A,H30B), O31(H31A,H31B), O32(H32A,H32B)
8.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C10(H10), C12(H12), C14(H14), C19(H19), C21(H21),
 C23(H23), C26(H26), C28(H28), C30(H30), C35(H35), C37(H37), C39(H39), C42(H42),
  C44(H44), C46(H46)
;
_shelx_res_checksum              89131
_shelx_hkl_checksum              7580
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'