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_1540645
_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         'C30 H32 N6 O8 Y, Cl, C2 H3 N'
_chemical_formula_sum            'C32 H35 Cl N7 O8 Y'
_chemical_formula_weight         770.03
_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   mixed
_audit_creation_date             2015-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.085(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2901(9)
_cell_length_b                   15.4666(11)
_cell_length_c                   18.7780(13)
_cell_measurement_temperature    100
_cell_volume                     3514.3(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.978
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22907
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_min         2.265
_exptl_absorpt_coefficient_mu    1.794
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         7924
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0690P)^2^+0.7250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5547
_reflns_number_total             7924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cifs.cif
_cod_data_source_block           2015ncs0277
_cod_database_code               1540645
_shelxl_version_number           2014-1
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.855
_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
 O7-H7
 0.85 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 C29-H7
 1.909553 with sigma of 0.02
 Y1-H7
 2.896379 with sigma of 0.02
 C30-H8
 1.899201 with sigma of 0.02
 Y1-H8
 2.903724 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C7(H7A), C2(H2A), C1(H1), C21(H21), C18(H18), C11(H11),
 C23(H23), C15(H15), C10(H10), C25(H25), C16(H16), C9(H9), C24(H24), C5(H5A),
 C19(H19), C4(H4)
3.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              37690
_shelx_hkl_checksum              58674
_olex2_submission_special_instructions 'No special instructions were received'