Solution and solid state structures and magnetism of a series of linear trinuclear compounds with a hexacoordinate Ln(III) and two terminal Ni(II) centers.
Comba, Peter; Enders, Markus; Großhauser, Michael; Hiller, Markus; Müller, Dennis; Wadepohl, Hubert; Dalton transactions (Cambridge, England : 2003) 46 (2016) 138–149; doi:10.1039/c6dt03488h

data_7041285
_publ_section_title
;
 Solution and solid state structures and magnetism of a series of linear
 trinuclear compounds with a hexacoordinate Ln(III) and two terminal
 Ni(II) centers.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              138
_journal_page_last               149
_journal_paper_doi               10.1039/c6dt03488h
_journal_volume                  46
_journal_year                    2016
_chemical_formula_moiety         'C66 H84 Dy N6 Ni2 O12, Cl O4'
_chemical_formula_sum            'C66 H84 Cl Dy N6 Ni2 O16'
_chemical_formula_weight         1532.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mg82
_audit_creation_date
;
'Mon Sep 07 15:41:26 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-03-07 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3859(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.89637(9)
_cell_length_b                   22.41000(15)
_cell_length_c                   23.03847(16)
_cell_measurement_reflns_used    67343
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.0010
_cell_measurement_theta_min      3.5640
_cell_volume                     6646.67(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details
;
  1 omega   -3.00   91.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000   60.0000 188

  2 omega    4.00   36.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000 -120.0000 64

  3 omega    1.00   77.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000  -90.0000 152

  4 omega    1.00   29.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000   60.0000 56

  5 omega    4.00   39.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000  150.0000 70

  6 omega   -4.00   21.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   80.0000   86.8579 50

  7 omega   -4.00   21.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   79.0000 -112.8448 50

  8 omega  -40.00   59.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000   21.0959 198

  9 omega  -43.00   59.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000 -156.7113 204

 10 omega   18.00   48.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   19.0000 -150.0000 60

 11 omega   -3.00   81.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000  -60.0000 168

 12 omega    6.00   32.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000   60.0000 52

 13 omega   41.00   68.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000   60.0000 54

 14 omega  -43.00   59.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -79.0000  -56.2127 204

 15 omega  -43.00   15.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000  141.8705 116

 16 omega  -43.00   59.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -79.0000   95.1560 204

 17 omega   18.00   60.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000  141.8705 84

 18 omega   32.00   60.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000 -102.8920 56

 19 omega  -43.00   -1.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000 -102.8920 84

 20 omega    6.00   96.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000  -60.0000 180

 21 omega   -5.00   24.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   80.0000   86.8579 58

 22 omega   -4.00   25.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   79.0000 -112.8448 58

 23 omega  -43.00   57.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000  -60.0000 200

 24 omega  -42.00  -12.50   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -57.0000   90.0000 59

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0106737000
_diffrn_orient_matrix_UB_12      -0.0305227000
_diffrn_orient_matrix_UB_13      0.0058569000
_diffrn_orient_matrix_UB_21      -0.0366372000
_diffrn_orient_matrix_UB_22      -0.0083239000
_diffrn_orient_matrix_UB_23      -0.0227404000
_diffrn_orient_matrix_UB_31      0.0397435000
_diffrn_orient_matrix_UB_32      0.0005172000
_diffrn_orient_matrix_UB_33      -0.0200073000
_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  0.0537
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            222510
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.827
_diffrn_reflns_theta_min         3.220
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    1.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light violet'
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             3156
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     840
_refine_ls_number_reflns         23387
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+4.8793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20243
_reflns_number_total             23387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03488h2.cif
_cod_data_source_block           co_mg82
_cod_depositor_comments
'Adding full bibliography for 7041276--7041289.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7041285
_audit_block_refno               2518
_audit_block_usercomment         'MG521, block, light violet'
_chemical_oxdiff_formula         'C66 H84 Cl1 Dy1 N6 Ni2 O16'
_chemical_oxdiff_usercomment     'MG521, block, light violet'
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.717
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl-O51 \\sim Cl-O54 \\sim Cl-O53 \\sim Cl-O52
 with sigma of 0.02
 O51-O52 \\sim O51-O53 \\sim O51-O54 \\sim O52-O53 \\sim O52-O54 \\sim O53-O54
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C101(H10A,H10B), C102(H10C,H10D), C103(H10E,H10F), C104(H10G,H10H), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C116(H11G,H11H), C125(H12G,H12H),
 C201(H20A,H20B), C202(H20C,H20D), C203(H20E,H20F), C204(H20G,H20H), C205(H20I,
 H20J), C206(H20K,H20L), C207(H20M,H20N), C216(H21G,H21H), C225(H22G,H22H)
3.b Me refined with riding coordinates:
 C214(H21A,H21B,H21C)
3.c Aromatic/amide H refined with riding coordinates:
 C111(H111), C113(H113), C120(H120), C122(H122), C129(H129), C131(H131),
 C211(H211), C213(H213), C220(H220), C222(H222), C229(H229), C231(H231)
3.d Idealised Me refined as rotating group:
 C114(H11A,H11B,H11C), C115(H11D,H11E,H11F), C123(H12A,H12B,H12C), C124(H12D,
 H12E,H12F), C132(H13A,H13B,H13C), C133(H13D,H13E,H13F), C215(H21D,H21E,H21F),
 C223(H22A,H22B,H22C), C224(H22D,H22E,H22F), C232(H23A,H23B,H23C), C233(H23D,
 H23E,H23F)
;
_shelx_res_checksum              54667
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.89605(8)
_cell_oxdiff_length_b            22.41673(18)
_cell_oxdiff_length_c            23.03221(15)
_cell_oxdiff_angle_alpha         90.0107(6)
_cell_oxdiff_angle_beta          93.3896(5)
_cell_oxdiff_angle_gamma         89.9905(6)
_cell_oxdiff_volume              6646.67(8)
_cell_oxdiff_measurement_reflns_used 67343