New Lanthanide (III) Coordination Polymers: Synthesis, Structural Features, and Catalytic Activity in CO2 Fixation
Xu, Cong; Liu, Yan; Wang, Li; Ma, Jingxin; Yang, Lizi; Pan, Fu-Xing; Kirillov, Alexander M.; Liu, Wei-Sheng; Dalton Trans.  (2017) –; doi:10.1039/C7DT03574H

data_7044528
_publ_section_title
;
 New Lanthanide (III) Coordination Polymers: Synthesis, Structural
 Features, and Catalytic Activity in CO2 Fixation
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03574H
_journal_year                    2017
_chemical_formula_moiety         'C34 H24 N4 O9 Tm, Cl'
_chemical_formula_sum            'C34 H24 Cl N4 O9 Tm'
_chemical_formula_weight         836.95
_chemical_name_common            Tm-Bcpi-Cl
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc14964s
_audit_creation_date             2015-02-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-27 deposited with the CCDC.
2017-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                82.848(6)
_cell_angle_beta                 68.734(8)
_cell_angle_gamma                68.687(8)
_cell_formula_units_Z            2
_cell_length_a                   10.3347(10)
_cell_length_b                   11.8348(8)
_cell_length_c                   14.1006(11)
_cell_measurement_reflns_used    5942
_cell_measurement_temperature    294.58(10)
_cell_measurement_theta_max      28.4410
_cell_measurement_theta_min      3.5900
_cell_volume                     1497.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.58(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   22.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   57.0000   30.0000 54

  2 omega  -24.00   39.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000 -120.0000 63

  3 omega  -19.00   24.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000   60.0000 43

  4 omega  -38.00   36.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -19.0000   90.0000 74

  5 omega  -38.00   16.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000   60.0000 36

  6 omega   -7.00   53.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   77.0000  -30.0000 40

  7 omega   43.00   68.50   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000 -180.0000 17

  8 omega  -33.00   18.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -77.0000 -150.0000 34

  9 omega   22.00   55.00   1.5000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -99.0000 -150.0000 22
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0176719000
_diffrn_orient_matrix_UB_12      0.0175275000
_diffrn_orient_matrix_UB_13      -0.0518196000
_diffrn_orient_matrix_UB_21      0.0457706000
_diffrn_orient_matrix_UB_22      -0.0607329000
_diffrn_orient_matrix_UB_23      -0.0149628000
_diffrn_orient_matrix_UB_31      -0.0611853000
_diffrn_orient_matrix_UB_32      -0.0119603000
_diffrn_orient_matrix_UB_33      -0.0024012000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12279
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.36
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.120
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'hydrothermal method'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.066
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         5882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0614
_reflns_number_gt                5345
_reflns_number_total             5882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt03574h2.cif
_cod_data_source_block           xuc0106
_cod_database_code               7044528
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C0AA(H0AA), C27(H27), C10(H10), C13(H13), C4(H4), C26(H26), C16(H16),
 C25(H25), C33(H33), C12(H12), C20(H20), C6(H6), C9(H9), C30(H30), C29(H29),
 C3(H3), C23(H23), C7(H7), C21(H21), C15(H15), C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'