Metal‒Organic Frameworks Containing (Alkynyl)Gold Functionalities: A Comparative Evaluation of Solvent-Assisted Linker Exchange,de NovoSynthesis, and Post-synthesis Modification
Madrahimov, Sherzod T.; Atesin, Tulay A.; Karagiaridi, Olga; Sarjeant, Amy A.; Farha, Omar K.; Hupp, Joseph T.; Nguyen, SonBinh T.; Crystal Growth & Design 14 (2014) 6320–; doi:10.1021/cg501066s

data_4512226
_publ_section_title
;
 Metal--Organic Frameworks Containing (Alkynyl)Gold Functionalities: A
 Comparative Evaluation of Solvent-Assisted Linker Exchange,de
 NovoSynthesis, and Post-synthesis Modification
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6320
_journal_paper_doi               10.1021/cg501066s
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C47 H24 Br2 N2 O8 Zn2'
_chemical_formula_sum            'C47 H24 Br2 N2 O8 Zn2'
_chemical_formula_weight         1035.24
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_Hall           '-P 2y'
_space_group_name_H-M_alt        'P 1 2/m 1'
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2014-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.169(12)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.270(3)
_cell_length_b                   15.803(2)
_cell_length_c                   16.274(3)
_cell_measurement_reflns_used    2489
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.684
_cell_measurement_theta_min      3.914
_cell_volume                     2875.7(10)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.547
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0700
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_Laue_measured_fraction_full 0.547
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6582
_diffrn_reflns_point_group_measured_fraction_full 0.547
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         51.223
_diffrn_reflns_theta_min         5.084
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.502
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.4724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0987 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.6299.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.598
_exptl_crystal_description       block
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2967
_refine_ls_number_restraints     201
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1459P)^2^+1.6857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2383
_refine_ls_wR_factor_ref         0.2556
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1826
_reflns_number_total             2967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg501066s_si_003.cif
_cod_data_source_block           n2412
_cod_depositor_comments          'Adding full bibliography for 4512226.cif.'
_cod_database_code               4512226
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.847
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C10-H10 = C11-H11
 0.95 with sigma of 0.001
 N1-C14 \\sim C13-C14 \\sim C12-C13 \\sim C12-C11 \\sim C11-C10 \\sim N1-C10
\\sim C13-C16
 with sigma of 0.02
 C14-C16 \\sim C12-C16
 with sigma of 0.02
 N1-C13 \\sim C14-C12 \\sim C13-C11 \\sim C12-C10 \\sim C11-N1 \\sim C10-C14
 with sigma of 0.02
 H10-N1 \\sim H11-C10 \\sim H10-C11 \\sim H11-C12
 with sigma of 0.02
3. Restrained planarity
 N1, C10, C11, C12, C13, C14
 with sigma of 0.1
4. 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
5. Others
 Fixed Sof: H10(0.25) H11(0.25) H15A(0.5) H15B(0.5) C16(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C14(H14)
;
_smtbx_masks_special_details
;
The solvent masking procedure in Olex2 was used to remove
the electronic contributions from disordered solvent as well
as the AuPR3 moiety which could not be located from residual
density maps.

Total solvent accessible volume / cell = 2087.4 Ang^3 [72.6%]
Total electron count / cell = 267.3
;
_shelx_res_checksum              62374
_shelx_hkl_checksum              8047