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_1540643
_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 H35 Cl2 Gd2 N9 O9, Cl'
_chemical_formula_sum            'C42 H35 Cl3 Gd2 N9 O9'
_chemical_formula_weight         1230.64
_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
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.982(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.218(3)
_cell_length_b                   20.386(4)
_cell_length_c                   20.455(4)
_cell_measurement_reflns_used    1606
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.7890
_cell_measurement_theta_min      4.1680
_cell_volume                     5800(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
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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)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.714
_diffrn_measured_fraction_theta_max 0.732
_diffrn_measurement_details
;
  1 omega  -85.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.1295  -38.0000  -60.0000 88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0366565000
_diffrn_orient_matrix_UB_12      -0.0152564000
_diffrn_orient_matrix_UB_13      -0.0137843000
_diffrn_orient_matrix_UB_21      0.0189944000
_diffrn_orient_matrix_UB_22      -0.0147200000
_diffrn_orient_matrix_UB_23      0.0312164000
_diffrn_orient_matrix_UB_31      -0.0303850000
_diffrn_orient_matrix_UB_32      -0.0274048000
_diffrn_orient_matrix_UB_33      -0.0094525000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.1212
_diffrn_reflns_laue_measured_fraction_full 0.714
_diffrn_reflns_laue_measured_fraction_max 0.732
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11110
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.732
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.651
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.456
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48748
_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    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.611
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         7486
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.098
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0735P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1576
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4625
_reflns_number_total             7486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cifs.cif
_cod_data_source_block           el529
_cod_original_cell_volume        5799.5(18)
_cod_database_code               1540643
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         C65H85Gd2Cl3N20O20
_reflns_odcompleteness_completeness 70.95
_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. Uiso/Uaniso restraints and constraints
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(N9) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.2
Uanis(Cl2) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.2
Uanis(Cl3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 C32, N9, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 N8(H8), N2(H2), N5(H5), C16(H16), C21(H21), C7(H7), C19(H19), C15(H15),
 C35(H35), C18(H18), C27(H27), C29(H29), C11(H11), C37(H37), C39(H39), C2(H2A),
 C30(H30), C26(H26), C12(H12), C13(H13), C4(H4), C38(H38), C25(H25), C32(H32),
 C5(H5A), C33(H33)
4.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C14(H14A,H14B,H14C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              44776
_shelx_hkl_checksum              34687
_olex2_submission_special_instructions 'No special instructions were received'