Cinnamic acid derivative rare-earth dinuclear complexes and one-dimensional architectures: synthesis, characterization and magnetic properties.
Khalfaoui, Ouafa; Beghidja, Adel; Long, Jérôme; Boussadia, Ahlem; Beghidja, Chahrazed; Guari, Yannick; Larionova, Joulia; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3943–3952; doi:10.1039/c7dt00326a

data_7042196
_publ_section_title
;
 Cinnamic acid derivative rare-earth dinuclear complexes and
 one-dimensional architectures: synthesis, characterization and magnetic
 properties.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3943
_journal_page_last               3952
_journal_paper_doi               10.1039/c7dt00326a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C62 H61.94 Dy2 O20 S0.99, C3 H7 N O'
_chemical_formula_sum            'C65 H68.94 Dy2 N O21 S0.99'
_chemical_formula_weight         1556.89
_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_block_doi                 10.5517/ccdc.csd.cc1nbw84
_audit_creation_date             2016-11-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.31 svn.r3340 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-01-26 deposited with the CCDC.
2017-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                92.555(6)
_cell_angle_beta                 116.958(5)
_cell_angle_gamma                98.755(5)
_cell_formula_units_Z            2
_cell_length_a                   15.0687(17)
_cell_length_b                   15.4141(17)
_cell_length_c                   16.0754(19)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      2.87
_cell_measurement_theta_min      26.70
_cell_volume                     3261.9(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            52779
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.348
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.380
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.585
_exptl_crystal_description       block
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.335
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         12944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0478P)^2^+6.4429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9151
_reflns_number_total             12944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00326a2.cif
_cod_data_source_block           FM108
_cod_depositor_comments
'Adding full bibliography for 7042193--7042199.cif.'
_cod_database_code               7042196
_shelx_estimated_absorpt_t_max   0.870
_shelx_estimated_absorpt_t_min   0.797
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Others
 Fixed Sof: S1A(0.66) S1B(0.33) H61A(0.66) H61B(0.66) H61C(0.66) H61D(0.33)
 H61E(0.33) H61F(0.33) H62A(0.66) H62B(0.66) H62C(0.66) H62D(0.33) H62E(0.33)
 H62F(0.33)
3.a Rotating group:
 O20(H20A,H20B)
3.b Me refined with riding coordinates:
 C61(H61A,H61B,H61C), C61(H61D,H61E,H61F), C62(H62A,H62B,H62C), C62(H62D,H62E,
 H62F)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C15(H15),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C25(H25), C27(H27), C28(H28),
  C29(H29), C32(H32), C33(H33), C35(H35), C37(H37), C38(H38), C39(H39),
 C42(H42), C43(H43), C45(H45), C47(H47), C48(H48), C49(H49), C52(H52), C53(H53),
  C55(H55), C57(H57), C58(H58), C59(H59), C63(H63)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C20(H20C,H20D,H20E), C30(H30A,H30B,H30C), C40(H40A,H40B,
 H40C), C50(H50A,H50B,H50C), C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C65(H65A,
 H65B,H65C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'