Conformation-directing chiral groups in bis(naphthaldiminato)nickel(ii) complexes: a rare example with 16 crystallographically independent units (Z′)
Ganadu, Maria Luisa; Demitri, Nicola; Zangrando, Ennio; CrystEngComm 20 (2018) 6122–; doi:10.1039/C8CE01089G

data_7231564
_publ_section_title
;
 Conformation-directing chiral groups in bis(naphthaldiminato)nickel(ii)
 complexes: a rare example with 16 crystallographically independent units
 (Z&#x2032;)
;
_journal_issue                   40
_journal_name_full               CrystEngComm
_journal_page_first              6122
_journal_paper_doi               10.1039/C8CE01089G
_journal_volume                  20
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C34 H40 N2 Ni O2'
_chemical_formula_sum            'C34 H40 N2 Ni O2'
_chemical_formula_weight         567.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-07-03 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.51(3)
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   18.579(4)
_cell_length_b                   31.710(6)
_cell_length_c                   40.968(8)
_cell_measurement_reflns_used    6455
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.75
_cell_measurement_theta_min      1.54
_cell_volume                     24113(8)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics    'Ortep3 for Windows (Farrugia,1997)'
_computing_publication_material  'Wingx Version 2013.3 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         'Elettra Synchrotron, Trieste (Italy)'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            270431
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.964
_diffrn_reflns_theta_min         0.490
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'W. Kabsch, Acta Cryst. D (2010)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       needle
_exptl_crystal_F_000             9664
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 55240 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0150(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     5745
_refine_ls_number_reflns         143030
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+1.4951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.897
_reflns_Friedel_fraction_max     0.817
_reflns_number_gt                132498
_reflns_number_total             143030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01089g2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7231563--7231564.cif.'
_cod_database_code               7231564
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              24215