Hybrid materials based on novel 2D lanthanide coordination polymers covalently bonded to amine-modified SBA-15 and MCM-41: assembly, characterization, structural features, thermal and luminescence properties.
Wang, Jun; Dou, Wei; Kirillov, Alexander M.; Liu, Weisheng; Xu, Cailing; Fang, Ran; Yang, Lizi; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18610–18621; doi:10.1039/c6dt03558b

data_7041037
_publ_section_title
;
 Hybrid materials based on novel 2D lanthanide coordination polymers
 covalently bonded to amine-modified SBA-15 and MCM-41: assembly,
 characterization, structural features, thermal and luminescence
 properties.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18610
_journal_page_last               18621
_journal_paper_doi               10.1039/c6dt03558b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C54 H43 N O21 Tb2'
_chemical_formula_sum            'C54 H43 N O21 Tb2'
_chemical_formula_weight         1359.73
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-10-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-09-09 deposited with the CCDC.
2016-10-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.8013(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.95347(19)
_cell_length_b                   34.1449(11)
_cell_length_c                   18.8756(4)
_cell_measurement_reflns_used    6716
_cell_measurement_temperature    295.42(10)
_cell_measurement_theta_max      28.4080
_cell_measurement_theta_min      3.4580
_cell_volume                     5114.8(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.42(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  -50.00  -24.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -38.0000  -90.0000 26

  2 omega  -17.00   25.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000   30.0000 42

  3 omega  -37.00    8.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416  -57.0000   30.0000 45

  4 omega  -49.00   33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416  -19.0000   60.0000 82

  5 omega  -70.00  -44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -77.0000   90.0000 26

  6 omega   37.00   97.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       20.7416  178.0000    0.0000 60
;
_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      -0.0096494000
_diffrn_orient_matrix_UB_12      0.0141936000
_diffrn_orient_matrix_UB_13      -0.0274233000
_diffrn_orient_matrix_UB_21      0.0083317000
_diffrn_orient_matrix_UB_22      -0.0148823000
_diffrn_orient_matrix_UB_23      -0.0257365000
_diffrn_orient_matrix_UB_31      -0.0884579000
_diffrn_orient_matrix_UB_32      -0.0029449000
_diffrn_orient_matrix_UB_33      -0.0019594000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22969
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.30
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.378
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         9004
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+16.5376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                7422
_reflns_number_total             9004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt03558b2.cif
_cod_data_source_block           wangj0422
_cod_depositor_comments
'Adding full bibliography for 7041036--7041037.cif.'
_cod_database_code               7041037
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H79A,H79B} of C79, {H7AA,H7AB} of C7AA, {H70A,H70B} of
  C70, {H83A,H83B} of C83, {H69A,H69B} of C69, All C(H,H,H) groups, All O(H)
  groups
 At 1 times of:
  {H8A,H8B} of C8
2. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O1BA) \\sim Ueq, Uanis(O1AA)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(O1AA) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C0AA) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: H8A(0.6) H8B(0.4) O9(0.6) O12(0.4)
4.a Riding coordinates:
 C8(H8A), C8(H8B)
4.b Secondary CH2 refined with riding coordinates:
 C70(H70A,H70B), C83(H83A,H83B), C69(H69A,H69B), C79(H79A,H79B), C7AA(H7AA,H7AB)
4.c Aromatic/amide H refined with riding coordinates:
 C6AA(H6AA), C2BA(H2BA), C23(H23), C24(H24), C30(H30), C37(H37), C42(H42),
 C86(H86), C64(H64), C85(H85), C2AA(H2AA), C3AA(H3AA), C5BA(H5BA), C9AA(H9AA),
 C8AA(H8AA), C7BA(H7BA), C4BA(H4BA), C17(H17), C19(H19), C11(H11), C20(H20),
 C8BA(H8BA), C4(H4), C7(H7), C3(H3)
4.d Idealised Me refined as rotating group:
 C1AA(H1AB,H1AC,H1AD), C4AA(H4AA,H4AB,H4AC)
4.e Idealised tetrahedral OH refined as rotating group:
 O1AA(H1AA)
;
_olex2_date_sample_data_collection 2015-04-24
_olex2_submission_special_instructions 'No special instructions were received'