Chirality at metal and helical ligand folding in optical isomers of chiral bis(naphthaldiminato)nickel(ii) complexes.
Enamullah, Mohammed; Quddus, Mohammad Abdul; Hasan, Mohammad Rezabul; Pescitelli, Gennaro; Berardozzi, Roberto; Makhloufi, Gamall; Vasylyeva, Vera; Janiak, Christoph; Dalton transactions (Cambridge, England : 2003) 45 (2015) 667–680; doi:10.1039/c5dt03940a

data_7037104
_publ_section_title
;
 Chirality at metal and helical ligand folding in optical isomers of
 chiral bis(naphthaldiminato)nickel(ii) complexes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              667
_journal_page_last               680
_journal_paper_doi               10.1039/c5dt03940a
_journal_volume                  45
_journal_year                    2015
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C38 H32 N2 Ni O2'
_chemical_formula_sum            'C38 H32 N2 Ni O2'
_chemical_formula_weight         607.36
_chemical_name_systematic
;
bis{(S)-N-phenylethyl-2-oxo-1-naphthaldiminato-\k^2^N,O}nickel(II)
;
_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
_audit_update_record
;
2015-06-05 deposited with the CCDC.
2015-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.192(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5328(9)
_cell_length_b                   15.2970(16)
_cell_length_c                   20.560(2)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.13
_cell_measurement_theta_min      2.35
_cell_volume                     2998.1(5)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'DIAMOND (Crystal Impact, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25081
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.225
_diffrn_reflns_theta_min         1.659
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.9285
_exptl_absorpt_correction_T_min  0.7004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Sheldrick, G. M. (2012) SADABS. Bruker AXS Inc., 
Madison, Wisconsin, USA. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 4159 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.040(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         10664
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0363P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0945
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.970
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                9694
_reflns_number_total             10664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03940a2.cif
_cod_data_source_block           nir33a_1messung
_cod_depositor_comments
'Adding full bibliography for 7037103--7037104.cif.'
_cod_database_code               7037104
_shelx_estimated_absorpt_t_min   0.700
_shelx_estimated_absorpt_t_max   0.928
_shelxl_version_number           2014-3
_shelx_res_checksum              96456