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_7037103
_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{(R)-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                 90.146(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5282(16)
_cell_length_b                   15.355(3)
_cell_length_c                   20.655(4)
_cell_measurement_reflns_used    7779
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.97
_cell_volume                     3021.9(10)
_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      95(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa APEX-II CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.1028
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28227
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.972
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 1996)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.335
_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          0.072
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 3394 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         12217
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0281P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.697
_reflns_Friedel_fraction_full    0.829
_reflns_Friedel_fraction_max     0.750
_reflns_number_gt                9892
_reflns_number_total             12217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03940a2.cif
_cod_data_source_block           Enam_NiR12
_cod_depositor_comments
'Adding full bibliography for 7037103--7037104.cif.'
_cod_database_code               7037103
_shelx_estimated_absorpt_t_min   0.953
_shelx_estimated_absorpt_t_max   0.956
_shelxl_version_number           2014-3
_shelx_res_checksum              11726