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_7046501
_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 Sm4)'
_chemical_formula_sum            'C44 H43 Cl4 N14 O13 Pd2 Sm'
_chemical_formula_weight         1480.87
_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                   10.1010(6)
_cell_length_b                   40.7504(15)
_cell_length_c                   15.1414(10)
_cell_measurement_reflns_used    6434
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      73.6230
_cell_measurement_theta_min      4.3040
_cell_volume                     6232.5(6)
_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_temperature      103(2)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega  -48.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8048   29.0000  -36.0000 83

  2 omega   46.00  145.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316 -165.0000  -61.0000 99

  3 omega   33.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -29.0000  162.0000 58

  4 omega  101.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   97.0000   90.0000 77

  5 omega  -39.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8048   38.0000 -120.0000 71

  6 omega -117.00  -86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8048 -165.0000  -61.0000 31

  7 omega    2.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.8048  -99.0000  -90.0000 81

  8 omega   34.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000 -150.0000 56

  9 omega   95.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  125.0000 -180.0000 81

 10 omega  106.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  125.0000  120.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            22154
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        64.997
_diffrn_reflns_theta_max         64.997
_diffrn_reflns_theta_min         4.340
_exptl_absorpt_coefficient_mu    13.716
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.992
_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_colour_primary    yellow
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             2924
_exptl_crystal_size_max          0.1116
_exptl_crystal_size_mid          0.0671
_exptl_crystal_size_min          0.0629
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.176
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0889
_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^)+(0.0500P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2009
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4222
_reflns_number_total             5175
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01288a2.cif
_cod_data_source_block           1_sq_sq
_cod_depositor_comments
'Adding full bibliography for 7046501--7046503.cif.'
_cod_database_code               7046501
_shelx_shelxl_version_number     2016/6
_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. Uiso/Uaniso restraints and constraints
C27 \\sim C9 \\sim C8 \\sim C7 \\sim C6 \\sim C5: within 0.01A with sigma of
3.8 and sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
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(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5)
 C9(0.5) H9(0.5) O3(0.5) H19C(0.5) H19D(0.5) H19A(0.5) H19B(0.5) C22(0.5)
 C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5) C26(0.5) H26(0.5) C27(0.5)
 H27(0.5) C28(0.5) O6(0.5) C29(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19C,H19D), C19(H19A,H19B), C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27)
4.c Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9), C23(C24,C25,C26,C27,C28)
;
_shelx_res_checksum              63545
_shelx_fab_checksum              77050
_olex2_submission_special_instructions 'No special instructions were received'