Optimal Binding of Acetylene to a Nitro-Decorated Metal-Organic Framework.
Duong, Thien D.; Sapchenko, Sergey A.; da Silva, Ivan; Godfrey, Harry G. W.; Cheng, Yongqiang; Daemen, Luke L.; Manuel, Pascal; Ramirez-Cuesta, Anibal J; Yang, Sihai; Schröder, Martin; Journal of the American Chemical Society 140 (2018) 16006–16009; doi:10.1021/jacs.8b08504

data_4133099
_publ_section_title
;
 Optimal Binding of Acetylene to a Nitro-Decorated Metal-Organic
 Framework.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16006
_journal_page_last               16009
_journal_paper_doi               10.1021/jacs.8b08504
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.11(C252 H117 Cu18 N18 O126)'
_chemical_formula_sum            'C28 H13 Cu2 N2 O14'
_chemical_formula_weight         728.48
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-07-22 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   18.3933(6)
_cell_length_b                   18.3933(6)
_cell_length_c                   52.3346(18)
_cell_measurement_reflns_used    11997
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3780
_cell_measurement_theta_min      4.3630
_cell_volume                     15333.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            40584
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.510
_diffrn_reflns_theta_min         3.248
_exptl_absorpt_coefficient_mu    1.060
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over a multifaceted crystal model
Empirical absorption correction using spherical harmonics,  implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.710
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3285
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.149
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       0.00017(6)
_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   1.517
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         3817
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.582
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0857
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3166
_refine_ls_wR_factor_ref         0.3301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3292
_reflns_number_total             3817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08504_si_002.cif
_cod_data_source_block           tddabb_sq
_cod_original_cell_volume        15333.5(11)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4133099
_shelx_estimated_absorpt_t_max   0.858
_shelx_estimated_absorpt_t_min   0.746
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O6-O5
 2.1 with sigma of 0.02
 O3-N1 = O4-N1
 1.2 with sigma of 0.005
 O3-O4
 2.08 with sigma of 0.02
 O4-N1 = O3-N1 = O6-N2 = O5-N2
 1.3 with sigma of 0.01
 O6-C8 = O5-C8
 2.5 with sigma of 0.02
 N1-C10
 1.4 with sigma of 0.05
 O4-C10 \\sim C10-O3
 with sigma of 0.002
 C12-C6 \\sim C13-C6 \\sim C10-C12 \\sim C13-C8 \\sim C8-C11 \\sim C10-C11
 with sigma of 0.02
3. Restrained planarity
 C12, C6, C5, C4
 with sigma of 0.1
 C5, C6, C13, C8
 with sigma of 0.1
 C6, C13, C8, C11
 with sigma of 0.1
 C8, N2, O5, O6
 with sigma of 0.002
 C6, C12, C10, C11
 with sigma of 0.1
 C12, C10, N1, C11
 with sigma of 0.1
 O4, O3, N1, C10
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O5 \\sim N2 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
O4 \\sim N1 \\sim O3 \\sim O5 \\sim N2 \\sim O6: within 2A with sigma of 0.002
and sigma for terminal atoms of 0.004
5. Rigid body (RIGU) restrains
 C11, C8, C10, C12, C13, C6, C5, C4, C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C13(0.5) H13(0.5) C12(0.5) H12(0.5) N1(0.25) O4(0.25) O3(0.25)
 N2(0.25) O5(0.25) O6(0.25) C8(0.5) H8(0.25) C10(0.5) H10(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C13(H13), C12(H12), C8(H8), C10(H10)
;
_shelx_res_checksum              61585
_shelx_hkl_checksum              74225
_shelx_fab_checksum              27558
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id MFM-102-NO2
_olex2_submission_special_instructions 'No special instructions were received'