Enhancing the magnetic performance of pyrazine-N-oxide bridged dysprosium chains through controlled variation of ligand coordination modes.
Ji, Xiao-Qin; Xiong, Jin; Sun, Rong; Ma, Fang; Sun, Hao-Ling; Zhang, Yi-Quan; Gao, Song; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7048–7055; doi:10.1039/d1dt00635e

data_7707093
_publ_section_title
;
 Enhancing the magnetic performance of pyrazine-N-oxide bridged dysprosium
 chains through controlled variation of ligand coordination modes.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7048
_journal_page_last               7055
_journal_paper_doi               10.1039/d1dt00635e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C27 H26 Br2 Cl2 Dy2 N8 O9, C H4 O'
_chemical_formula_sum            'C28 H30 Br2 Cl2 Dy2 N8 O10'
_chemical_formula_weight         1194.32
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-08 deposited with the CCDC.	2021-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.261(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5998(8)
_cell_length_b                   16.0132(12)
_cell_length_c                   24.1951(19)
_cell_measurement_reflns_used    4076
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      27.8010
_cell_measurement_theta_min      3.4520
_cell_volume                     3713.3(5)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3127
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     18.00  52.00   1.00    5.80    --   23.13 -99.00  90.00   34
  2  \w      6.00 128.00   1.00    5.80    --   23.13 -19.00 -90.00  122
  3  \w     47.00 127.00   1.00    5.80    --   23.13 178.00 -30.00   80
;
_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      -0.0019092000
_diffrn_orient_matrix_UB_12      -0.0438494000
_diffrn_orient_matrix_UB_13      0.0039397000
_diffrn_orient_matrix_UB_21      -0.0169601000
_diffrn_orient_matrix_UB_22      0.0061513000
_diffrn_orient_matrix_UB_23      0.0278456000
_diffrn_orient_matrix_UB_31      -0.0721141000
_diffrn_orient_matrix_UB_32      -0.0002788000
_diffrn_orient_matrix_UB_33      -0.0083361000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13914
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.32
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84438
_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            'clear light yellow'
_exptl_crystal_density_diffrn    2.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         7273
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0076P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                5733
_reflns_number_total             7273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt00635e2.cif
_cod_data_source_block           20161118a
_cod_depositor_comments
'Adding full bibliography for 7707093--7707094.cif.'
_cod_database_code               7707093
_chemical_oxdiff_formula         'C1 H1 O1 N1 Br1 Cl1 Dy1'
_reflns_odcompleteness_completeness 99.72
_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, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 O8-H8
 0.85 with sigma of 0.01
 O7-H7
 0.85 with sigma of 0.01
 C27-H6
 1.910545 with sigma of 0.02
 Dy1-H6
 2.873782 with sigma of 0.02
 C26-H8
 1.90401 with sigma of 0.02
 Dy2-H8
 2.899894 with sigma of 0.02
 C25-H7
 1.919363 with sigma of 0.02
 Dy2-H7
 3.095477 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N7) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C7(H7a), C10(H10), C24(H24), C22(H22), C15(H15), C18(H18), C6(H6a),
 C2(H2), C11(H11), C23(H23), C3(H3), C12(H12), C14(H14)
4.b Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C26(H26a,H26b,H26c), C25(H25a,H25b,H25c), C01G(H01a,H01b,
 H01c)
4.c Idealised tetrahedral OH refined as rotating group:
 O00N(H00N)
;
_olex2_date_sample_data_collection 2016-11-18
_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 1.427
_oxdiff_exptl_absorpt_empirical_full_min 0.826