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_1540644
_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         'C16 H20 Dy N5 O11'
_chemical_formula_sum            'C16 H20 Dy N5 O11'
_chemical_formula_weight         620.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                95.672(3)
_cell_angle_beta                 95.377(2)
_cell_angle_gamma                109.768(3)
_cell_formula_units_Z            4
_cell_length_a                   10.3419(3)
_cell_length_b                   14.5850(5)
_cell_length_c                   15.7309(5)
_cell_measurement_temperature    173
_cell_measurement_theta_max      61.0780
_cell_measurement_theta_min      4.5720
_cell_volume                     2201.46(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19968
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        61.091
_diffrn_reflns_theta_max         61.091
_diffrn_reflns_theta_min         4.015
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.7821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.00057(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         6718
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0310
_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^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5861
_reflns_number_total             6718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cifs.cif
_cod_data_source_block           el486c
_cod_original_cell_volume        2201.47(13)
_cod_database_code               1540644
_chemical_oxdiff_formula         Dy2C40H40N12O12Cl8
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O16-H16
 0.85 with sigma of 0.01
 O7-H7
 0.85 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 O15-H15
 0.85 with sigma of 0.01
 C32-H16
 1.876327 with sigma of 0.02
 Dy2-H16
 2.892671 with sigma of 0.02
 C15-H7
 1.90795 with sigma of 0.02
 Dy1-H7
 2.916123 with sigma of 0.02
 C16-H8
 1.874947 with sigma of 0.02
 Dy1-H8
 2.91521 with sigma of 0.02
 C31-H15
 1.864088 with sigma of 0.02
 Dy2-H15
 2.920947 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C13(H13), C17(H17), N2(H2), C20(H20), N5(H5A), C2(H2A), C18(H18),
 C26(H26), C21(H21), C12(H12), C25(H25), C4(H4), C1(H1), C23(H23), C7(H7A),
 C5(H5), C27(H27)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C16(H16A,H16B,
 H16C), C31(H31A,H31B,H31C), C15(H15A,H15B,H15C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'