Self-complementary nickel halides enable multifaceted comparisons of intermolecular halogen bonds: fluoride ligands <i>vs.</i> other halides.
Thangavadivale, Vargini; Aguiar, Pedro M.; Jasim, Naseralla A.; Pike, Sarah J.; Smith, Dan A.; Whitwood, Adrian C.; Brammer, Lee; Perutz, Robin N.; Chemical science 9 (2018) 3767–3781; doi:10.1039/c8sc00890f

data_1549115
_publ_section_title
;
 Self-complementary nickel halides enable multifaceted comparisons of
 intermolecular halogen bonds: fluoride ligands <i>vs.</i> other halides.
;
_journal_issue                   15
_journal_name_full               'Chemical science'
_journal_page_first              3767
_journal_page_last               3781
_journal_paper_doi               10.1039/c8sc00890f
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C18 H30 F5 I Ni P2'
_chemical_formula_sum            'C18 H30 F5 I Ni P2'
_chemical_formula_weight         588.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_symmetry_space_group_name_Hall  'I 2y'
_symmetry_space_group_name_H-M   'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2014-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2018-02-23 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.434(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8920(5)
_cell_length_b                   11.3325(4)
_cell_length_c                   12.9439(5)
_cell_measurement_reflns_used    2721
_cell_measurement_temperature    111(2)
_cell_measurement_theta_max      31.4640
_cell_measurement_theta_min      3.5820
_cell_volume                     1154.19(10)
_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
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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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      111(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega   59.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6365   57.0000   30.0000 36

  2 omega   16.00   41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6365  -57.0000 -120.0000 25

  3 omega    6.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6365  -99.0000    0.0000 63

  4 omega  -20.00   61.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6365  -99.0000 -120.0000 81

  5 omega  -39.00   96.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6365    0.0000 -150.0000 135

  6 omega   63.00  101.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6365  178.0000 -120.0000 38

  7 omega   -2.00   31.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       26.6365   77.0000  120.0000 33
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0679480000
_diffrn_orient_matrix_UB_12      -0.0259017000
_diffrn_orient_matrix_UB_13      -0.0312029000
_diffrn_orient_matrix_UB_21      0.0192951000
_diffrn_orient_matrix_UB_22      -0.0556201000
_diffrn_orient_matrix_UB_23      0.0229863000
_diffrn_orient_matrix_UB_31      -0.0561751000
_diffrn_orient_matrix_UB_32      0.0121637000
_diffrn_orient_matrix_UB_33      0.0389430000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4467
_diffrn_reflns_point_group_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.849
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.115
_diffrn_reflns_theta_min         2.926
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89095
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       needle
_exptl_crystal_F_000             588
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.3444
_exptl_crystal_size_mid          0.0676
_exptl_crystal_size_min          0.0297
_refine_diff_density_max         1.791
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.019(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         4467
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0295P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.645
_reflns_Friedel_fraction_full    0.793
_reflns_Friedel_fraction_max     0.699
_reflns_number_gt                4037
_reflns_number_total             4467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00890f2.cif
_cod_data_source_block           1pF_VT_200K_rnp1416a_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1549107--1549121.cif.'
_cod_original_cell_volume        1154.19(9)
_cod_database_code               1549115
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C18 H30 F5 I1 Ni1 P2'
_chemical_oxdiff_usercomment     'Vargini's Ni(F)(PEt3)2(C6F4I) 110K'
_diffrn_oxdiff_twin_integration_method simultaneous
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5,H), C7(HC,HD), C9(HE,HF)
2.b Idealised Me refined as rotating group:
 C6(HA,HB,H6), C10(HG,HH,HI), C8(H8,HJ,HK)
;
_shelx_res_checksum              39485
_shelx_hkl_checksum              22399
_olex2_submission_special_instructions 'No special instructions were received'