Synthesis and crystal structure of bis(μ2-acetato-κ2 O:O′)-di(ethanol)-bis{μ2-5-(N,N′-diethylamine)-5′-methoxyl-2,2′-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato-κ6 O:O,N,N,O′:O′}trinickel(II) – ethanol – acetonitrile (1/2/2), C58H86Ni3N8O18
Zong-Li, Ren; Xiao-Xin, An; Ling-Zhi, Liu; Peng-Fei, Lan; Wen-Kui, Dong; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 495–497; doi:10.1515/ncrs-2017-0388

data_8106195
_publ_section_title
;
 Synthesis and crystal structure of bis(\m2-acetato-\k2
 O:O&#x2032;)-di(ethanol)-bis{\m2-5-(N,N&#x2032;-diethylamine)-5&#x2032;-methoxyl-2,2&#x2032;-[ethylenediyldioxybis(nitrilomethylidyne)]diphenolato-\k6
 O:O,N,N,O&#x2032;:O&#x2032;}trinickel(II) -- ethanol -- acetonitrile
 (1/2/2), C58H86Ni3N8O18
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              495
_journal_page_last               497
_journal_paper_doi               10.1515/ncrs-2017-0388
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C50 H68 N6 Ni3 O16, 2(C2 H6 O), 2(C2 H3 N)'
_chemical_formula_sum            'C58 H86 N8 Ni3 O18'
_chemical_formula_weight         1359.48
_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
_cell_angle_alpha                109.620(7)
_cell_angle_beta                 101.234(7)
_cell_angle_gamma                114.469(6)
_cell_formula_units_Z            1
_cell_length_a                   11.4561(8)
_cell_length_b                   13.1859(8)
_cell_length_c                   13.5063(11)
_cell_measurement_reflns_used    3207
_cell_measurement_temperature    173.69(10)
_cell_measurement_theta_max      28.0320
_cell_measurement_theta_min      3.8380
_cell_volume                     1611.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      173.69(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   -5.00   79.00   1.2000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8979   38.0000   90.0000 70

  2 omega   -5.00   25.00   1.2000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  -99.0000  -90.0000 25

  3 omega  -19.00   13.40   1.2000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  -99.0000 -120.0000 27

  4 omega  -16.00   11.60   1.2000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  -99.0000   60.0000 23

  5 omega  -44.00   65.20   1.2000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8979  -19.0000 -120.0000 91

  6 omega   35.00   97.40   1.2000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8979 -178.0000 -150.0000 52

  7 omega   35.00   96.20   1.2000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.8979  178.0000  -60.0000 51
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0171660000
_diffrn_orient_matrix_UB_12      0.0051408000
_diffrn_orient_matrix_UB_13      0.0555291000
_diffrn_orient_matrix_UB_21      -0.0280656000
_diffrn_orient_matrix_UB_22      -0.0659503000
_diffrn_orient_matrix_UB_23      -0.0240377000
_diffrn_orient_matrix_UB_31      0.0661235000
_diffrn_orient_matrix_UB_32      0.0094164000
_diffrn_orient_matrix_UB_33      0.0017138000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11648
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.954
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6323
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0496P)^2^+1.0235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1315
_reflns_number_gt                4833
_reflns_number_total             6323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0388_suppl.cif
_cod_data_source_block           d608
_cod_original_cell_volume        1611.1(2)
_cod_database_code               8106195
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O8-H8
 0.85 with sigma of 0.01
 Ni1-H8
 2.654842 with sigma of 0.02
 C24-H8
 1.892678 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C25') \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: H24A(0.65) H24B(0.65) H24C(0.35) H24D(0.35) C25(0.65) H25A(0.65)
 H25B(0.65) H25C(0.65) C25'(0.35) H25D(0.35) H25E(0.35) H25F(0.35)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C18(H18A,H18B), C20(H20A,H20B), C24(H24A,H24B),
 C24(H24C,H24D), C27(H27A,H27B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C11(H11), C14(H14), C16(H16), C17(H17)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C25'(H25D,H25E,H25F), C26(H26A,H26B,H26C),
 C28(H28A,H28B,H28C)
5.d Idealised tetrahedral OH refined as rotating group:
 O9(H9)
;
_olex2_date_sample_data_collection 2015-01-19
_olex2_submission_special_instructions 'No special instructions were received'