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_7041287
_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 Er N6 Ni2 O12, Cl O4'
_chemical_formula_sum            'C66 H84 Cl Er N6 Ni2 O16'
_chemical_formula_weight         1537.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                co_mg66
_audit_creation_date             2016-04-04
_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                 106.643(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.090(9)
_cell_length_b                   21.331(9)
_cell_length_c                   17.493(7)
_cell_measurement_reflns_used    8014
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.31
_cell_measurement_theta_min      2.26
_cell_volume                     7182(5)
_computing_cell_refinement
;
SAINT (see _computing_data_reduction). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction
'SAINT (Bruker AXS, 1997-2013),SADABS-2014_4 (Sheldrick and Bruker AXS, 1997-2014)'
_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      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            91595
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.473
_diffrn_reflns_theta_min         1.909
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.780
_exptl_absorpt_correction_T_max  0.3012
_exptl_absorpt_correction_T_min  0.2570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (see _computing_data_reduction)
;
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3164
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.140
_refine_diff_density_max         3.329
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         12409
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0591P)^2^+21.1536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10847
_reflns_number_total             12409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03488h2.cif
_cod_data_source_block           co_mg66_sq
_cod_depositor_comments
'Adding full bibliography for 7041276--7041289.cif.'
_cod_original_cell_volume        7183(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7041287
_audit_block_refno               2177
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.685
_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-O52 \\sim Cl-O53 \\sim Cl-O54
 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
 Cl, O51, O52, O53, O54
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Cl(0.5) O51(0.5) O52(0.5) O53(0.5) O54(0.5)
5.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)
5.b Aromatic/amide H refined with riding coordinates:
 C111(H111), C113(H113), C120(H120), C122(H122), C129(H129), C131(H131)
5.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              25133
_shelx_fab_checksum              6053
_olex2_submission_special_instructions 'No special instructions were received'