Dinuclear Lanthanide (III) Coordination Polymers in a Domino Reaction
Loukopoulos, Edward; Griffiths, Kieran; Akien, Geoffrey; Kourkoumelis, Nikolaos; Abdul-Sada, Alaa; Kostakis, George; Inorganics 3 (2015) 448–; doi:10.3390/inorganics3040448

data_1540641
_publ_section_title
;
 Dinuclear Lanthanide (III) Coordination Polymers in a Domino Reaction
;
_journal_issue                   4
_journal_name_full               Inorganics
_journal_page_first              448
_journal_paper_doi               10.3390/inorganics3040448
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety         'C14.63 H14.27 N4 O7 Y, 0.68(C2 H6 O)'
_chemical_formula_sum            'C16 H18.37 N4 O7.68 Y'
_chemical_formula_weight         478.56
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6954(4)
_cell_length_b                   14.3307(6)
_cell_length_c                   18.2161(4)
_cell_measurement_reflns_used    7320
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.4960
_cell_measurement_theta_min      4.8560
_cell_volume                     3836.2(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -14.00   65.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -57.0000 -120.0000 79

  2 omega   40.00   70.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000 -180.0000 30

  3 omega   38.00   70.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000 -120.0000 32

  4 omega   43.00   72.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 29

  5 omega   40.00   66.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -30.0000 26

  6 omega   38.00   65.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -60.0000 27

  7 omega   38.00   64.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -90.0000 26

  8 omega   40.00  178.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000    0.0000  -60.0000 138

  9 omega  123.00  148.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -90.0000 25

 10 omega   98.00  148.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -30.0000 50

 11 omega   83.00  109.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -90.0000 26

 12 omega   51.00  142.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000 -150.0000 91

 13 omega   48.00   79.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -90.0000 31

 14 omega   40.00   70.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000 -150.0000 30

 15 omega   37.00   70.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000    0.0000 33

 16 omega   42.00   70.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000   30.0000 28

 17 omega   42.00   72.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   90.0000 30

 18 omega   43.00   68.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  120.0000 25

 19 omega   43.00   69.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  150.0000 26

 20 omega   38.00   64.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  120.0000 26

 21 omega   39.00   70.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000   60.0000 31

 22 omega   42.00  105.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000    0.0000 63

 23 omega   55.00  132.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -93.0000   70.1199 77

 24 omega   81.00  107.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  150.0000 26

 25 omega   98.00  123.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000   30.0000 25

 26 omega   73.00   98.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  -60.0000 25

 27 omega   62.00  127.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  178.0000 -120.0000 65

 28 omega   25.00  116.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000    0.0000 91

 29 omega    1.00   28.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -180.0000 27

 30 omega  -22.00   32.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 54

 31 omega  -16.00   36.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   60.0000 52

 32 omega  -73.00  -19.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500   57.0000  120.0000 54

 33 omega -102.00  -74.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000  -30.0000 28

 34 omega  -67.00  -15.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000 -180.0000 52

 35 omega -119.00  -40.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000  120.0000 79

 36 omega -112.00  -18.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000  150.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0191800000
_diffrn_orient_matrix_UB_12      -0.0990951000
_diffrn_orient_matrix_UB_13      -0.0289209000
_diffrn_orient_matrix_UB_21      0.1013130000
_diffrn_orient_matrix_UB_22      -0.0111914000
_diffrn_orient_matrix_UB_23      -0.0198606000
_diffrn_orient_matrix_UB_31      0.0189389000
_diffrn_orient_matrix_UB_32      -0.0401574000
_diffrn_orient_matrix_UB_33      0.0769435000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25890
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.620
_diffrn_reflns_theta_min         4.855
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
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    1.657
_exptl_crystal_description       plate
_exptl_crystal_F_000             1943
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.334
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3721
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+3.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2838
_reflns_number_total             3721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cifs.cif
_cod_data_source_block           el643b
_cod_database_code               1540641
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         Y2C30H30N10O10
_reflns_odcompleteness_completeness 99.92
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 C1-C2
 1.53 with sigma of 0.02
 C1-O1
 1.43 with sigma of 0.02
 C0AA-C1A
 1.43 with sigma of 0.02
 O005-C1A
 1.48 with sigma of 0.02
 O0-H0
 0.85 with sigma of 0.01
 C1A-H0
 2.019226 with sigma of 0.02
 Y001-H0
 3.100199 with sigma of 0.02
3. Rigid bond restraints
 C00M
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O005
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, O1, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O0, O005
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim O1 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O0 \\sim O005: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C1, O1, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0, O005
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O005(0.6832) H00A(0.6832) H00B(0.6832) O1(0.6832) H1(0.6832)
 C1(0.6832) H1A(0.6832) H1B(0.6832) C2(0.6832) H2A(0.6832) H2B(0.6832)
 H2C(0.6832) C1A(0.3168) H1AA(0.3168) H1AB(0.3168) C0AA(0.3168) H0AA(0.3168)
 H0AB(0.3168) H0AC(0.3168) O0(0.3168) H0(0.3168)
7.a Rotating group:
 O005(H00A,H00B)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C1A(H1AA,H1AB)
7.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P)
7.d Idealised Me refined as rotating group:
 C00Q(H00C,H00D,H00E), C2(H2A,H2B,H2C), C0AA(H0AA,H0AB,H0AC)
7.e Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'