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_7046503
_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 N32 O40 Pd8 Tb4)'
_chemical_formula_sum            'C44 H46 Cl4 N8 O14.5 Pd2 Tb'
_chemical_formula_weight         1432.41
_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                   10.1189(4)
_cell_length_b                   40.7335(17)
_cell_length_c                   15.0742(10)
_cell_measurement_reflns_used    4095
_cell_measurement_temperature    102.23(10)
_cell_measurement_theta_max      71.9550
_cell_measurement_theta_min      4.3200
_cell_volume                     6213.3(5)
_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      102.23(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details
;
  1 omega   16.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5548   43.0000  177.0000 99

  2 omega   95.00  178.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816   79.0000   -4.0000 83

  3 omega   37.00   97.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -43.0000   25.0000 60

  4 omega   78.00  172.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  150.0000   42.0000 94

  5 omega  -50.00   33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5548   38.0000  -60.0000 83

  6 omega  -50.00   33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5548   38.0000 -150.0000 83

  7 omega   36.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5548 -150.0000   -2.0000 78

  8 omega   37.00   98.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -45.0000 -180.0000 61

  9 omega   47.00   74.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -30.0000  -30.0000 27

 10 omega   38.00  109.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -94.0000   60.0000 71
;
_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      -0.0162534000
_diffrn_orient_matrix_UB_12      -0.0127654000
_diffrn_orient_matrix_UB_13      0.0956715000
_diffrn_orient_matrix_UB_21      0.0800770000
_diffrn_orient_matrix_UB_22      0.0294608000
_diffrn_orient_matrix_UB_23      0.0348029000
_diffrn_orient_matrix_UB_31      -0.1284289000
_diffrn_orient_matrix_UB_32      0.0199519000
_diffrn_orient_matrix_UB_33      0.0097072000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24751
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.922
_diffrn_reflns_theta_min         5.265
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.221
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.844
_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    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             2828
_exptl_crystal_size_max          0.0994
_exptl_crystal_size_mid          0.0634
_exptl_crystal_size_min          0.0616
_refine_diff_density_max         1.466
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6261
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0987
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3151
_reflns_number_total             6261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01288a2.cif
_cod_data_source_block           3_sq
_cod_depositor_comments
'Adding full bibliography for 7046501--7046503.cif.'
_cod_original_cell_volume        6213.3(6)
_cod_original_formula_sum        'C44 H46 Cl4 N8 O14.50 Pd2 Tb'
_cod_database_code               7046503
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Sm1 C1 N1 O1 Pd1 H1 Cl1'
_reflns_odcompleteness_completeness 99.89
_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
 C26-O2
 1.36 with sigma of 0.01
 O1-C26
 1.36 with sigma of 0.01
 C24-C26
 1.5 with sigma of 0.01
 C23-O4
 1.36 with sigma of 0.01
 O3-C23
 1.36 with sigma of 0.01
 O4-C18
 2.8 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C19 \\sim C16 \\sim C28 \\sim C25: within 0.01A with sigma of 3.8 and sigma for
terminal atoms of 0.01
C27 \\sim C14B \\sim C12: within 0.01A with sigma of 3.8 and sigma for terminal
atoms of 0.01
Uanis(C25) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C28)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C24) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C14A) \\sim Ueq, Uanis(C14B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C23) \\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
 Sof(C14B)=Sof(H14B)=1-FVAR(1)
 Sof(C14A)=Sof(H14A)=FVAR(1)
 Fixed Sof: H3BC(0.5) H3BD(0.5) H3AA(0.5) H3AB(0.5) C27(0.5) H27(0.5) C24(0.5)
 C28(0.5) H28(0.5) C25(0.5) H25(0.5) C19(0.5) O4(0.5) C23(0.5) O1(0.5) C26(0.5)
 C22(0.5) H22(0.5) C21(0.5) C18(0.5) H18(0.5) C20(0.5) H20(0.5) C17(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3BC,H3BD), C3(H3AA,H3AB), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C11(H11), C12(H12), C14B(H14B), C27(H27), C28(H28), C25(H25),
 C16(H16), C6(H6), C13(H13), C15(H15), C14A(H14A), C22(H22), C18(H18), C20(H20)
5.c Fitted hexagon refined as free rotating group:
 C14B(C27,C24,C28,C25,C19), C16(C8,C6,C13,C9,C15), C14A(C22,C21,C18,C20,C17)
;
_shelx_res_checksum              6383
_shelx_fab_checksum              10249
_ins_header
;
TITL SY-7 in Pnna 
REM Pnna (#52, found as Pnan in a-cb setting)
CELL 1.54184  10.118859  40.733550  15.074250  90.0000  90.0000  90.0000
ZERR    4.00   0.000446   0.001704   0.001030   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 H N O Cl Pd Sm
UNIT 4.00 4.00 4.00 4.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'