Structural diversity of luminescent lanthanide metal‒organic frameworks based on a V-shaped ligand
He, Yan-Fei; Chen, Di-Ming; Xu, Hang; Cheng, Peng; CrystEngComm 17 (2015) 2471–; doi:10.1039/C4CE02380C

data_7219172
_publ_section_title
;
 Structural diversity of luminescent lanthanide metal--organic frameworks
 based on a V-shaped ligand
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              2471
_journal_paper_doi               10.1039/C4CE02380C
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C45 H35 Eu2 N O18'
_chemical_formula_sum            'C45 H34 Eu2 N O18'
_chemical_formula_weight         1180.65
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-08-12
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2014-10-20 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.446(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4187(6)
_cell_length_b                   28.0878(14)
_cell_length_c                   16.7579(11)
_cell_measurement_reflns_used    6597
_cell_measurement_temperature    133.8(2)
_cell_measurement_theta_max      28.6620
_cell_measurement_theta_min      3.4450
_cell_volume                     4373.2(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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_temperature      133.8(2)
_diffrn_detector_area_resol_mean 16.2116
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega   34.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372 -178.0000  150.0000 55

  2 omega  -48.00   43.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372  -37.0000  -60.0000 91

  3 omega  -12.00   28.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000 -120.0000 40

  4 omega    7.00   37.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0372   77.0000  -60.0000 30

  5 omega  -40.00  -10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.9747   57.0000 -180.0000 30
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0001478000
_diffrn_orient_matrix_UB_12      -0.0223766000
_diffrn_orient_matrix_UB_13      0.0197138000
_diffrn_orient_matrix_UB_21      -0.0180527000
_diffrn_orient_matrix_UB_22      -0.0114220000
_diffrn_orient_matrix_UB_23      -0.0380161000
_diffrn_orient_matrix_UB_31      0.0741351000
_diffrn_orient_matrix_UB_32      -0.0027918000
_diffrn_orient_matrix_UB_33      -0.0020705000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18345
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.922
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2324
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.254
_refine_diff_density_min         -1.535
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         7618
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+38.2968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                6104
_reflns_number_total             7618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02380c2.cif
_cod_data_source_block           p140630a
_cod_depositor_comments
'Adding full bibliography for 7219168--7219173.cif.'
_cod_database_code               7219172
_chemical_oxdiff_formula         C1H1O1N1EU1
_chemical_oxdiff_usercomment     6-25-EU4
_reflns_odcompleteness_completeness 99.77
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C2-N2 = N2-C1
 1.45 with sigma of 0.01
 H1B-H62B
 2.2 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C9 \\sim N2 \\sim C2 \\sim C1 \\sim O60: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C9) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Rotating group:
 O61(H61A,H61B), O62(H62A,H62B)
5.b Ternary CH refined with riding coordinates:
 C9(H9)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C11(H11), C12(H12), C14(H14), C15(H15),
 C23(H23), C24(H24), C26(H26), C27(H27), C30(H30), C31(H31), C33(H33), C34(H34),
  C42(H42), C43(H43), C45(H45), C46(H46), C49(H49), C50(H50), C52(H52), C53(H53)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'