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_7041289
_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 Lu N6 Ni2 O12, Cl O4'
_chemical_formula_sum            'C66 H84 Cl Lu N6 Ni2 O16'
_chemical_formula_weight         1545.23
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mg67
_audit_creation_date
;
'Tue Sep 30 16:43:12 2014'
;
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Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-04 deposited with the CCDC.
2016-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.771(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5007(7)
_cell_length_b                   23.1939(5)
_cell_length_c                   18.0326(5)
_cell_measurement_reflns_used    13341
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      23.8970
_cell_measurement_theta_min      3.5590
_cell_volume                     7785.4(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
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_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 0.997
_diffrn_measurement_details
;
  1 omega    4.00   50.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  154.3876 92

  2 omega  -31.00   50.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -80.0000  -25.5584 162

  3 omega   17.00   50.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  -66.2298 66

  4 omega   -2.00   87.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000 -150.0000 178

  5 omega   -4.00   23.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000 -150.0000 54

  6 omega  -36.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   60.0000 170

  7 omega   -5.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -150.0000 108

  8 omega  -12.00   89.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000    0.0000 202

  9 omega    6.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000    0.0000 86

 10 omega  -45.00  -18.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -120.0000 54

 11 omega   13.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -120.0000 72

 12 omega   15.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   90.0000 68

 13 omega   -8.00   88.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000  120.0000 192

 14 omega    0.00   83.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  -60.0000 166

 15 omega  -43.00  -14.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 58

 16 omega  -48.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -90.0000 194

 17 omega  -18.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   30.0000 134

 18 omega   17.00   49.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 64

 19 omega  -47.00  -19.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  154.3876 56

;
_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      -0.0370737000
_diffrn_orient_matrix_UB_12      0.0066837000
_diffrn_orient_matrix_UB_13      -0.0208502000
_diffrn_orient_matrix_UB_21      0.0021563000
_diffrn_orient_matrix_UB_22      -0.0035595000
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_diffrn_orient_matrix_UB_31      -0.0086057000
_diffrn_orient_matrix_UB_32      -0.0296149000
_diffrn_orient_matrix_UB_33      -0.0001145000
_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  0.1540
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            157031
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.404
_diffrn_reflns_theta_min         3.283
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    1.833
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       needle
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.018
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         15932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+18.8988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11968
_reflns_number_total             15932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03488h2.cif
_cod_data_source_block           co_mg67_sq
_cod_depositor_comments
'Adding full bibliography for 7041276--7041289.cif.'
_cod_original_cell_volume        7785.4(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7041289
_audit_block_refno               2193
_audit_block_usercomment         'MG427, needle, colourless'
_chemical_oxdiff_formula         'C66 H84 Cl N6 O16 Ni2 Lu'
_chemical_oxdiff_usercomment     'MG427, needle, colourless'
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.771
_reflns_odcompleteness_completeness 99.76
_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.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)
2.b 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)
2.c 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), C214(H21A,H21B,H21C),
 C215(H21D,H21E,H21F), C223(H22A,H22B,H22C), C224(H22D,H22E,H22F), C232(H23A,
 H23B,H23C), C233(H23D,H23E,H23F)
;
_shelx_res_checksum              84627
_shelx_fab_checksum              78038
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            20.4931(5)
_cell_oxdiff_length_b            23.2043(4)
_cell_oxdiff_length_c            18.0318(5)
_cell_oxdiff_angle_alpha         89.9762(18)
_cell_oxdiff_angle_beta          114.776(3)
_cell_oxdiff_angle_gamma         89.9828(18)
_cell_oxdiff_volume              7785.4(3)
_cell_oxdiff_measurement_reflns_used 13341