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_1549109
_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_absolute_configuration ad
_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             2014-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 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                 94.392(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8675(5)
_cell_length_b                   11.3291(3)
_cell_length_c                   12.9347(6)
_cell_measurement_reflns_used    3697
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.2660
_cell_measurement_theta_min      3.1250
_cell_volume                     1149.51(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
;
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      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measurement_details
;
  1 omega -101.00  -64.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1392 -178.0000   30.0000 37

  2 omega  -17.00   77.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455   19.0000   30.0000 94

  3 omega  -42.00   61.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455    0.0000  -30.0000 103

  4 omega  -20.00   68.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455  -99.0000    0.0000 88

  5 omega   -4.00   97.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455   77.0000 -180.0000 101

  6 omega  -42.00   48.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455  -57.0000 -180.0000 90

  7 omega  -46.00  100.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455    0.0000 -180.0000 146
;
_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      0.0008588000
_diffrn_orient_matrix_UB_12      0.0268449000
_diffrn_orient_matrix_UB_13      -0.0494513000
_diffrn_orient_matrix_UB_21      0.0683320000
_diffrn_orient_matrix_UB_22      -0.0372185000
_diffrn_orient_matrix_UB_23      -0.0118535000
_diffrn_orient_matrix_UB_31      -0.0592822000
_diffrn_orient_matrix_UB_32      -0.0426073000
_diffrn_orient_matrix_UB_33      -0.0208729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.887
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5693
_diffrn_reflns_point_group_measured_fraction_full 0.874
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.348
_diffrn_reflns_theta_min         2.931
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.367
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.689
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.702
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.2226
_exptl_crystal_size_mid          0.1261
_exptl_crystal_size_min          0.0726
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 882 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.087(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2011
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0345P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0595
_reflns_Friedel_coverage         0.865
_reflns_Friedel_fraction_full    0.859
_reflns_Friedel_fraction_max     0.830
_reflns_number_gt                1952
_reflns_number_total             2011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00890f2.cif
_cod_data_source_block           1pF_rnp1332a_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1549107--1549121.cif.'
_cod_database_code               1549109
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C18 H30 F5 I1 Ni1 P2'
_chemical_oxdiff_usercomment     'Vargini's Ni(F)(PEt3)2(C6F4I)'
_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. Uiso/Uaniso restraints and constraints
Uanis(F1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B)
3.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              65201
_shelx_hkl_checksum              88896
_olex2_submission_original_sample_id rnp1332
_olex2_submission_special_instructions 'No special instructions were received'