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_7228557
_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         'C78 H66 Dy4 N18 O22'
_chemical_formula_sum            'C78 H66 Dy4 N18 O22'
_chemical_formula_weight         2257.49
_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                104.640(3)
_cell_angle_beta                 93.446(3)
_cell_angle_gamma                92.084(3)
_cell_formula_units_Z            1
_cell_length_a                   10.5185(4)
_cell_length_b                   12.0831(4)
_cell_length_c                   16.6476(4)
_cell_measurement_reflns_used    7252
_cell_measurement_temperature    212(30)
_cell_measurement_theta_max      73.0810
_cell_measurement_theta_min      3.7880
_cell_volume                     2040.53(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41k (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      N~2~
_diffrn_ambient_temperature      212(30)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9952
_diffrn_measured_fraction_theta_max 0.9952
_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    -65.00  -8.00   1.00    2.00    --  -41.74 125.00-120.00   57
  2  \w   -116.00  -1.00   1.00    2.00    --  -41.74 -19.00 -30.00  115
  3  \w     23.00  60.00   1.00    2.00    --   41.74-125.00-120.00   37
  4  \w     49.00  78.00   1.00    2.00    --   41.74-125.00-180.00   29
  5  \w     69.00 121.00   1.00    4.00    --  107.19-125.00-180.00   52
  6  \w     71.00 133.00   1.00    4.00    --  107.19 -77.00 -30.00   62
  7  \w     95.00 133.00   1.00    4.00    --  107.19 -45.00 -30.00   38
  8  \w     71.00 109.00   1.00    4.00    --  107.19 -94.00 -30.00   38
  9  \w     65.00 118.00   1.00    4.00    --  107.19-125.00   0.00   53
 10  \w     41.00  98.00   1.00    2.00    --   41.74-125.00   0.00   57
 11  \w     34.00 119.00   1.00    4.00    --  107.19 -45.00 120.00   85
 12  \w     68.00 140.00   1.00    4.00    --  107.19 -77.00 150.00   72
 13  \w     78.00 166.00   1.00    4.00    --  107.19  63.00  39.00   88
 14  \w     35.00 133.00   1.00    4.00    --  107.19 -45.00-120.00   98
 15  \w     35.00  61.00   1.00    4.00    --  107.19-125.00-180.00   26
 16  \w     27.00 168.00   1.00    4.00    --  107.19   0.00  30.00  141
 17  \w     27.00  58.00   1.00    4.00    --  107.19 -94.00 150.00   31
 18  \w   -111.00 -33.00   1.00    2.00    --  -41.74 -37.00  90.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0619111000
_diffrn_orient_matrix_UB_12      -0.0972805000
_diffrn_orient_matrix_UB_13      -0.0611793000
_diffrn_orient_matrix_UB_21      0.1332395000
_diffrn_orient_matrix_UB_22      0.0541253000
_diffrn_orient_matrix_UB_23      0.0349485000
_diffrn_orient_matrix_UB_31      0.0021691000
_diffrn_orient_matrix_UB_32      -0.0708621000
_diffrn_orient_matrix_UB_33      0.0650455000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14340
_diffrn_reflns_theta_full        68.2384
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         7.45
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.8370
_exptl_crystal_description       block
_exptl_crystal_F_000             1064.3849
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.9048
_refine_diff_density_min         -1.7426
_refine_diff_density_rms         0.1372
_refine_ls_d_res_high            0.8301
_refine_ls_d_res_low             5.9459
_refine_ls_goodness_of_fit_ref   1.0244
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    58
_refine_ls_number_parameters     553
_refine_ls_number_reflns         7436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0244
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.0485
_refine_ls_shift/su_mean         0.0005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              14
_reflns_limit_k_min              -14
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                6396
_reflns_number_total             7436
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7ce00747g2.cif
_cod_data_source_block           151228a
_cod_database_code               7228557
_chemical_oxdiff_formula         'C1 H1 N1 O1 Dy1'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C12(H12), C13(H13), C14(H14), C28(H28), C29(H29), C30(H30), C26(H26),
 C25(H25), C9(H9), C10(H10), C17(H17), C18(H18), C19(H19), C20(H20), C5(H5),
 C1(H1), C3(H3), C7(H7), C23(H23), C33(H33), C2(H2)
2.b Idealised Me refined as rotating group:
 C34(H34a,H34b,H34c), C35(H35a,H35b,H35c), C37(H37a,H37b,H37c), C39(H39a,H39b,
 H39c)
;
_olex2_date_sample_data_collection 2015-12-28
_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 1.615
_oxdiff_exptl_absorpt_empirical_full_min 0.758