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_7041279
_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 N6 Nd Ni2 O12, 2(Cl O4)'
_chemical_formula_sum            'C66 H84 Cl2 N6 Nd Ni2 O20'
_chemical_formula_weight         1613.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      52
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mg62
_audit_creation_date
;
'Tue Oct 28 12:38:25 2014'
;
_audit_creation_method
;
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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.94563(15)
_cell_length_b                   25.5344(3)
_cell_length_c                   22.9043(3)
_cell_measurement_reflns_used    47829
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.7580
_cell_measurement_theta_min      3.6490
_cell_volume                     7571.22(16)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34k (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,16:31:05)
;
_computing_data_reduction
;
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)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 0.971
_diffrn_measurement_details
;
  1 omega   24.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  -95.9662 52

  2 omega  -29.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000    6.0138 158

  3 omega   22.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000   51.8131 56

  4 omega  -47.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  102.7857 194

  5 omega  -20.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -80.0000  154.3390 140

  6 omega  -11.00   15.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000   30.0000 52

  7 omega   14.00   65.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  -90.0000 102

  8 omega    2.00   28.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  150.0000 52

  9 omega   24.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -150.0000 50

 10 omega  -12.00   88.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000 -180.0000 200

 11 omega   23.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -60.0000 52

 12 omega   -6.00   19.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   38.0000   60.0000 50

 13 omega   24.00   69.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   38.0000   60.0000 90

 14 omega    3.00   87.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  -30.0000 168

 15 omega   15.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -120.0000 68

 16 omega   -3.00   85.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000   60.0000 176

 17 omega  -33.00   -1.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000   30.0000 64

 18 omega   -8.00   18.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 52

 19 omega   21.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 56

 20 omega  -14.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   19.0000 -150.0000 146

 21 omega  -46.00    0.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000  -95.9662 92

 22 omega  -12.00   68.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000  120.0000 160

;
_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      -0.0098789000
_diffrn_orient_matrix_UB_12      0.0263028000
_diffrn_orient_matrix_UB_13      -0.0082489000
_diffrn_orient_matrix_UB_21      -0.0393996000
_diffrn_orient_matrix_UB_22      -0.0086403000
_diffrn_orient_matrix_UB_23      -0.0192302000
_diffrn_orient_matrix_UB_31      -0.0367723000
_diffrn_orient_matrix_UB_32      0.0021883000
_diffrn_orient_matrix_UB_33      0.0228379000
_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  0.0484
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            163640
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.974
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.821
_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            'light violet'
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.087
_refine_diff_density_max         2.169
_refine_diff_density_min         -1.917
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         9766
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0671
_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^)+(0.0586P)^2^+43.3446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8982
_reflns_number_total             9766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03488h2.cif
_cod_data_source_block           co_mg62_sq
_cod_depositor_comments
'Adding full bibliography for 7041276--7041289.cif.'
_cod_original_cell_volume        7571.21(16)
_cod_database_code               7041279
_audit_block_refno               2169
_audit_block_usercomment         'MG424, irrgeluar, light violet'
_chemical_oxdiff_formula         'C66 H84 Cl N6 Nd Ni2 O16'
_chemical_oxdiff_usercomment     'MG424, irrgeluar, light violet'
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.775
_reflns_odcompleteness_completeness 99.65
_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
 Cl1-O53 \\sim Cl1-O54 \\sim Cl1-O52 \\sim Cl1-O51
 with sigma of 0.01
 O51-O52 \\sim O51-O53 \\sim O51-O54 \\sim O52-O53 \\sim O52-O54 \\sim O53-O54
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O53, Cl1, O52, O51, O54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.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)
4.b Aromatic/amide H refined with riding coordinates:
 C111(H111), C113(H113), C120(H120), C122(H122), C129(H129), C131(H131)
4.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)
;
_shelx_res_checksum              18363
_shelx_fab_checksum              47880
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.94541(18)
_cell_oxdiff_length_b            25.5402(4)
_cell_oxdiff_length_c            22.8995(3)
_cell_oxdiff_angle_alpha         89.9442(13)
_cell_oxdiff_angle_beta          89.9780(12)
_cell_oxdiff_angle_gamma         90.0040(12)
_cell_oxdiff_volume              7571.2(2)
_cell_oxdiff_measurement_reflns_used 47829