Detection of adsorbates on emissive MOF surfaces with X-ray photoelectron spectroscopy.
Yan, Jingjing; Carl, Alexander D.; Maag, Alex R.; MacDonald, John C.; Müller, Peter; Grimm, Ronald L.; Burdette, Shawn C.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4520–4529; doi:10.1039/c8dt04404j

data_7049217
_publ_section_title
;
 Detection of adsorbates on emissive MOF surfaces with X-ray photoelectron
 spectroscopy.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4520
_journal_page_last               4529
_journal_paper_doi               10.1039/c8dt04404j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C42 H34 N6 O8 Zn2'
_chemical_formula_sum            'C42 H34 N6 O8 Zn2'
_chemical_formula_weight         881.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2018-07-26 deposited with the CCDC.    2019-03-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.21(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.730(3)
_cell_length_b                   15.100(3)
_cell_length_c                   10.023(2)
_cell_measurement_reflns_used    3731
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.18
_cell_measurement_theta_min      2.46
_cell_volume                     2078.0(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11989
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.058
_diffrn_reflns_theta_min         2.005
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       Needle
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         2357
_refine_ls_number_restraints     865
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0844P)^2^+0.8442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1825
_reflns_number_total             2357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04404j2.cif
_cod_data_source_block           pm
_cod_depositor_comments
'Adding full bibliography for 7049217--7049218.cif.'
_cod_database_code               7049217
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C16-C17 = C16A-C17A
 1.55 with sigma of 0.02
3. Restrained planarity
 N1, C11, C12, C13, C14, C15, C16
 with sigma of 0.1
 N1A, C11A, C12A, C13A, C14A, C15A, C16A
 with sigma of 0.1
 N2, C21, C22, C23, C24, C25, C26, N3
 with sigma of 0.1
 N2A, C21A, C22A, C23A, C24A, C25A, C26A, N3A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(N1) = Uanis(N1A)
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. Same fragment restrains
{Zn1, N1A, C11A, C12A, C13A, C14A, C15A, C16A, C17A, N2A, C21A, C22A, C23A,
C24A, C25A, C26A, N3A} sigma for 1-2: 0.01, 1-3: 0.04
as
{Zn1, N1, C11, C12, C13, C14, C15, C16, C17, N2, C21, C22, C23, C24, C25, C26,
N3}
7. Others
 Sof(N1A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=
 Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=
 Sof(H17C)=Sof(H17D)=Sof(N2A)=Sof(H2A)=Sof(C21A)=Sof(C22A)=Sof(C23A)=Sof(H23A)=
 Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(N3A)=0.5*(1-
 FVAR(2))
 Sof(N1)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(C14)=Sof(H14)=
 Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=
 Sof(N2)=Sof(H2)=Sof(C21)=Sof(C22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)=
 Sof(H25)=Sof(C26)=Sof(H26)=Sof(N3)=0.5*FVAR(2)
8.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C16A(H16C,H16D), C17A(H17C,H17D)
8.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), N2(H2), C23(H23), C24(H24), C25(H25),
 C26(H26), C11A(H11A), C12A(H12A), C14A(H14A), C15A(H15A), N2A(H2A), C23A(H23A),
  C24A(H24A), C25A(H25A), C26A(H26A), C4(H4), C3(H3)
;
_shelx_res_checksum              81938
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'