6,6′-{[Ethane-1,2-diylbis(azaneylylidene)]bis(methaneylylidene)}bis[2-(hexyloxy)phenolato] Nickel(II)
Lukyanov, Daniil A.; Borisova, Anna S.; Levin, Oleg V.; Molbank 2020 (2020) M1174–; doi:10.3390/M1174

data_1559973
_publ_section_title
;
 6,6&#x2032;-{[Ethane-1,2-diylbis(azaneylylidene)]bis(methaneylylidene)}bis[2-(hexyloxy)phenolato]
 Nickel(II)
;
_journal_issue                   4
_journal_name_full               Molbank
_journal_page_first              M1174
_journal_paper_doi               10.3390/M1174
_journal_volume                  2020
_journal_year                    2020
_chemical_formula_moiety         'C28 H38 N2 Ni O4, C H2 Cl2'
_chemical_formula_sum            'C29 H40 Cl2 N2 Ni O4'
_chemical_formula_weight         610.24
_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     dual
_audit_creation_date             2020-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                97.065(3)
_cell_angle_beta                 101.868(3)
_cell_angle_gamma                93.363(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6002(3)
_cell_length_b                   13.6714(5)
_cell_length_c                   14.7436(5)
_cell_measurement_reflns_used    4450
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      28.7290
_cell_measurement_theta_min      3.0230
_cell_volume                     1482.24(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.71a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2096
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.897
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -38.00  42.00   1.00  120.00    --   20.13 -57.00 120.00   80
  2  \w    -48.00  40.00   1.00  120.00    --   20.13 -57.00   0.00   88
  3  \w     -7.00  26.00   1.00  120.00    --   20.13  77.00 120.00   33
  4  \w     -6.00  25.00   1.00  120.00    --   20.13  77.00   0.00   31
  5  \w     -5.00  34.00   1.00  120.00    --   20.13  77.00-120.00   39
  6  \w    -50.00  45.00   1.00  120.00    --   20.13 -38.00-120.00   95
  7  \w      9.00  51.00   1.00  120.00    --   20.13  57.00 -90.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0509173000
_diffrn_orient_matrix_UB_12      0.0414042000
_diffrn_orient_matrix_UB_13      0.0294114000
_diffrn_orient_matrix_UB_21      -0.0310825000
_diffrn_orient_matrix_UB_22      0.0307829000
_diffrn_orient_matrix_UB_23      -0.0342712000
_diffrn_orient_matrix_UB_31      -0.0748607000
_diffrn_orient_matrix_UB_32      0.0095802000
_diffrn_orient_matrix_UB_33      0.0205967000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.897
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11770
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.498
_diffrn_reflns_theta_min         2.749
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.71a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       prism
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0325P)^2^+0.5939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0759
_refine_ls_wR_factor_ref         0.0833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5469
_reflns_number_total             6749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            s5.cif
_cod_data_source_block           15823_bas001
_cod_database_code               1559973
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C28 H38 N2 Ni1 O4'
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.818
_reflns_odcompleteness_completeness 99.90
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00B), C00K(H00D,H00F), C00N(H00G,H00H), C00Q(H00K,H00L), C00R(H00N,
 H00Q), C00T(H00R,H00T), C00U(H00U,H00V), C00V(H0AA,H), C00W(H00W,H00X),
 C00X(H00Y,HA), C00Y(H00Z,HB), C010(H01A,H01B), C011(H01C,H01D)
2.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00E(H00E), C00I(H00I), C00J(H00J), C00M(H00M), C00O(H00O),
 C00P(H00P), C00S(H00S)
2.c Idealised Me refined as rotating group:
 C00Z(H00,HC,HD), C012(H01E,H01F,H01G)
;
_shelx_res_checksum              23723
_shelx_hkl_checksum              20392
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.127
_oxdiff_exptl_absorpt_empirical_full_min 0.881