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_7707094
_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         'C15 H14 Br Cl Dy N5 O4'
_chemical_formula_sum            'C15 H14 Br Cl Dy N5 O4'
_chemical_formula_weight         606.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                68.629(10)
_cell_angle_beta                 84.789(8)
_cell_angle_gamma                66.328(11)
_cell_formula_units_Z            2
_cell_length_a                   8.50540(10)
_cell_length_b                   10.29646(12)
_cell_length_c                   12.8339(11)
_cell_measurement_reflns_used    1618
_cell_measurement_temperature    100(20)
_cell_measurement_theta_max      25.9090
_cell_measurement_theta_min      3.8020
_cell_volume                     956.56(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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(20)
_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     17.00 105.00   1.00    2.70    --   23.13  57.00  60.00   88
  2  \w     35.00  60.00   1.00    2.70    --  -21.88 178.00-150.00   25
  3  \w    -20.00 101.00   1.00    2.70    --   23.13  37.00-150.00  121
  4  \w    -13.00  27.00   1.00    2.70    --  -21.88 -99.00-180.00   40
  5  \w    -36.00  64.00   1.00    2.70    --   23.13 -57.00 -90.00  100
;
_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      -0.0712762000
_diffrn_orient_matrix_UB_12      0.0413347000
_diffrn_orient_matrix_UB_13      -0.0400755000
_diffrn_orient_matrix_UB_21      0.0362684000
_diffrn_orient_matrix_UB_22      0.0536405000
_diffrn_orient_matrix_UB_23      -0.0285105000
_diffrn_orient_matrix_UB_31      0.0439386000
_diffrn_orient_matrix_UB_32      -0.0437220000
_diffrn_orient_matrix_UB_33      -0.0334410000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.1029
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5320
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.33
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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    2.105
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.370
_refine_diff_density_min         -1.383
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         3361
_refine_ls_number_restraints     222
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0500
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                2797
_reflns_number_total             3361
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1dt00635e2.cif
_cod_data_source_block           20170524f
_cod_depositor_comments
'Adding full bibliography for 7707093--7707094.cif.'
_cod_original_cell_volume        956.56(8)
_cod_database_code               7707094
_chemical_oxdiff_formula         'C1 H1 O1 N1 Br1 Dy1 Cl1'
_reflns_odcompleteness_completeness 99.67
_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. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 3.8A with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.02
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13)
3.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_olex2_date_sample_data_collection 2017-05-24
_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 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.643