Construction and magnetic study of two new dysprosium complexes with chain or tetranuclear structure
Yang, Jing; Ma, Fang; Deng, Xuebin; Sun, Hao-Ling; Zhang, Yiquan; CrystEngComm  (2017) –; doi:10.1039/C7CE00747G

data_7228556
_publ_section_title
;
 Construction and magnetic study of two new dysprosium complexes with
 chain or tetranuclear structure
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00747G
_journal_year                    2017
_chemical_formula_moiety         'C38 H34 Dy2 N12 O14, 2(C3 H7 N O)'
_chemical_formula_sum            'C44 H48 Dy2 N14 O16'
_chemical_formula_weight         1353.95
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2016-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-04-19 deposited with the CCDC.
2017-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                113.320(6)
_cell_angle_beta                 105.223(5)
_cell_angle_gamma                100.116(5)
_cell_formula_units_Z            1
_cell_length_a                   10.5498(5)
_cell_length_b                   11.5578(8)
_cell_length_c                   12.2337(8)
_cell_measurement_reflns_used    3636
_cell_measurement_temperature    298.54(10)
_cell_measurement_theta_max      26.9800
_cell_measurement_theta_min      3.8570
_cell_volume                     1254.24(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.6a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.54(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.8170
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -4.00  81.00   1.00    3.00    --   12.45  37.00   0.00   85
  2  \w     -1.00  30.00   1.00    3.00    --   12.45  37.00  90.00   31
  3  \w    -77.00  10.00   1.00    3.00    --  -11.20 -57.00  60.00   87
  4  \w      3.00  29.00   1.00    3.00    --  -11.20 -99.00-180.00   26
  5  \w    -37.00  61.00   1.00    3.00    --  -11.20  57.00-150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0314729000
_diffrn_orient_matrix_UB_12      0.0463797000
_diffrn_orient_matrix_UB_13      -0.0170055000
_diffrn_orient_matrix_UB_21      -0.0249707000
_diffrn_orient_matrix_UB_22      0.0480798000
_diffrn_orient_matrix_UB_23      0.0377192000
_diffrn_orient_matrix_UB_31      0.0614627000
_diffrn_orient_matrix_UB_32      0.0223344000
_diffrn_orient_matrix_UB_33      0.0538365000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_unetI/netI     0.1084
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10938
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         29.77
_diffrn_reflns_theta_min         3.35
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.6a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.7924
_exptl_crystal_description       block
_exptl_crystal_F_000             670.1173
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.7177
_refine_diff_density_min         -2.0723
_refine_diff_density_rms         0.2862
_refine_ls_d_res_high            0.7158
_refine_ls_d_res_low             6.0787
_refine_ls_goodness_of_fit_ref   0.9946
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    40
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5859
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9946
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.0027
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0116P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              12
_reflns_limit_k_min              -14
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4888
_reflns_number_total             5859
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7ce00747g2.cif
_cod_data_source_block           20160822a
_cod_original_cell_volume        1254.23(16)
_cod_database_code               7228556
_chemical_oxdiff_formula         'C1 H1 N1 O1 Dy1'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
2.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C7(H7), C5(H5), C1(H1), C3(H3), C9(H9), C2(H2), C10(H10), C14(H14),
 C13(H13), C12(H12), C20(H20)
2.b Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C22(H22a,H22b,H22c), C19(H19a,H19b,H19c), C18(H18a,H18b,
 H18c)
;
_olex2_date_sample_data_collection 2016-08-22
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.831