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_1540642
_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         'C42 H36 Cl2 Dy2 N9 O9, Cl'
_chemical_formula_sum            'C42 H36 Cl3 Dy2 N9 O9'
_chemical_formula_weight         1242.15
_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
_audit_creation_date             2015-10-08
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.857(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2871(3)
_cell_length_b                   19.9839(6)
_cell_length_c                   20.0637(7)
_cell_measurement_reflns_used    8597
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.8140
_cell_measurement_theta_min      3.6020
_cell_volume                     5606.2(3)
_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, 2015)'
_computing_structure_solution    'ShelXS (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 0.976
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
  1 omega  -89.00  -32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9733  178.0000 -120.0000 57

  2 omega  -31.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.9733   57.0000  150.0000 79

  3 omega   -1.00   56.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.7545  -99.0000 -120.0000 57
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0018170000
_diffrn_orient_matrix_UB_12      0.0338292000
_diffrn_orient_matrix_UB_13      -0.0108921000
_diffrn_orient_matrix_UB_21      -0.0446495000
_diffrn_orient_matrix_UB_22      0.0039433000
_diffrn_orient_matrix_UB_23      0.0097817000
_diffrn_orient_matrix_UB_31      0.0240130000
_diffrn_orient_matrix_UB_32      0.0099747000
_diffrn_orient_matrix_UB_33      0.0330259000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_laue_measured_fraction_full 0.976
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23213
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.721
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.840
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67374
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         11177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0616P)^2^+6.8047P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9122
_reflns_number_total             11177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cifs.cif
_cod_data_source_block           el508b
_cod_database_code               1540642
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         D2C60H60O4N10
_reflns_odcompleteness_completeness 98.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N8(H8), N5(H5), N2(H2), C12(H12), C36(H36), C22(H22), C8(H8A), C13(H13),
 C14(H14), C31(H31), C33(H33), C11(H11), C3(H3), C32(H32), C19(H19), C25(H25),
 C26(H26), C17(H17), C4(H4), C5(H5A), C18(H18), C42(H42), C41(H41), C39(H39),
 C28(H28), C27(H27), C40(H40)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C29(H29A,H29B,H29C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              18645
_shelx_hkl_checksum              99166
_olex2_submission_special_instructions 'No special instructions were received'