Tailoring the structure, pH sensitivity and catalytic performance in Suzuki-Miyaura cross-couplings of Ln/Pd MOFs based on the 1,1'-di(p-carboxybenzyl)-2,2'-diimidazole linker.
You, Li-Xin; Cui, Lan-Xin; Zhao, Bai-Bei; Xiong, Gang; Ding, Fu; Ren, Bao-Yi; Shi, Zhong-Liang; Dragutan, Ileana; Dragutan, Valerian; Sun, Ya-Guang; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8755–8763; doi:10.1039/c8dt01288a

data_7046502
_publ_section_title
;
 Tailoring the structure, pH sensitivity and catalytic performance in
 Suzuki-Miyaura cross-couplings of Ln/Pd MOFs based on the
 1,1'-di(p-carboxybenzyl)-2,2'-diimidazole linker.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8755
_journal_page_last               8763
_journal_paper_doi               10.1039/c8dt01288a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.25(C176 H128 Cl16 Eu4 N32 O40 Pd8)'
_chemical_formula_sum            'C44 H38 Cl4 Eu N8 O10.5 Pd2'
_chemical_formula_weight         1353.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-05-29 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1709(7)
_cell_length_b                   40.820(2)
_cell_length_c                   15.1189(12)
_cell_measurement_reflns_used    5868
_cell_measurement_temperature    101.98(18)
_cell_measurement_theta_max      75.4520
_cell_measurement_theta_min      4.3090
_cell_volume                     6277.0(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      101.98(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details
;
  1 omega  -11.00  122.20   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798   15.0000 -104.0000 444

  2 omega   54.00   88.80   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798 -112.0000  -70.0000 116

  3 omega   35.00  104.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816 -112.0000  -70.0000 230

  4 omega   46.00  123.10   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816 -142.0000 -142.0000 257

  5 omega   58.00  141.10   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816   15.0000 -104.0000 277

  6 omega  -37.00    9.20   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   38.0000 -150.0000 154

  7 omega  -49.00   32.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   38.0000  -30.0000 270

  8 omega   53.00   87.20   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -45.0000  -30.0000 114

  9 omega   34.00   86.20   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -30.0000   60.0000 174

 10 omega   40.00   74.80   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -30.0000  -60.0000 116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1351181000
_diffrn_orient_matrix_UB_12      -0.0153719000
_diffrn_orient_matrix_UB_13      -0.0199987000
_diffrn_orient_matrix_UB_21      -0.0618992000
_diffrn_orient_matrix_UB_22      -0.0344288000
_diffrn_orient_matrix_UB_23      0.0037704000
_diffrn_orient_matrix_UB_31      -0.0291204000
_diffrn_orient_matrix_UB_32      0.0018302000
_diffrn_orient_matrix_UB_33      -0.0998479000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21140
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.832
_diffrn_reflns_theta_min         4.332
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.632
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_description       block
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.0982
_exptl_crystal_size_mid          0.0681
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6132
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0840
_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^)+100.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4073
_reflns_number_total             6132
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01288a2.cif
_cod_data_source_block           2_sq_sq
_cod_depositor_comments
'Adding full bibliography for 7046501--7046503.cif.'
_cod_original_formula_sum        'C44 H38 Cl4 Eu N8 O10.50 Pd2'
_cod_database_code               7046502
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Pd1 Pr1 N1 C1 O1'
_shelx_estimated_absorpt_t_max   0.516
_shelx_estimated_absorpt_t_min   0.348
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C16-O3
 1.3 with sigma of 0.01
 C16-C20
 1.5 with sigma of 0.01
 O4-C16
 1.3 with sigma of 0.01
 C29-C27
 1.5 with sigma of 0.01
 O5_$1-C29
 1.3 with sigma of 0.01
 O6-C29
 1.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C25 \\sim C24 \\sim C23 \\sim C28 \\sim C27 \\sim C26 \\sim C29 \\sim O6:
within 0.01A with sigma of 3.8 and sigma for terminal atoms of 0.01
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C25) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H14C(0.5) H14D(0.5) O4(0.5) C16(0.5) C17(0.5)
 C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5) C21(0.5) H21(0.5) C22(0.5)
 H22(0.5) C23(0.5) H23(0.5) C24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5)
 C27(0.5) C28(0.5) H28(0.5) O6(0.5) C29(0.5)
5.a :
 N005(C1,C2,N008,C3), N006(C4,C5,N007,C6)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C14(H14C,H14D)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28)
5.d Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C17(C18,C19,C20,C21,C22), C23(C24,C25,C26,C27,C28)
;
_shelx_res_checksum              49813
_shelx_fab_checksum              18423
_ins_header
;
TITL SY-3 in Pnna 
REM Pnna (#52, found as Pnan in a-cb setting)
CELL 1.54184  10.170935  40.819757  15.118875  90.0000  90.0000  90.0000
ZERR    4.00   0.000718   0.002252   0.001224   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z 
SYMM -x+1/2, y+1/2,-z+1/2 
SYMM  x,-y+1/2,-z+1/2 
SFAC C N O Pd Pr
UNIT 4.00 4.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'