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_1549110
_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 F4 Ni P2'
_chemical_formula_sum            'C18 H30 F4 Ni P2'
_chemical_formula_weight         443.07
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-23 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.13398(18)
_cell_length_b                   8.13398(18)
_cell_length_c                   31.6136(10)
_cell_measurement_reflns_used    2396
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.8160
_cell_measurement_theta_min      3.5810
_cell_volume                     2091.61(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_details
;
  1 omega  -45.00   46.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4802  -37.0000  -90.0000 91

  2 omega    7.00   38.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       26.4802   19.0000  150.0000 31
;
_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      -0.0105988000
_diffrn_orient_matrix_UB_12      -0.0201935000
_diffrn_orient_matrix_UB_13      -0.0216575000
_diffrn_orient_matrix_UB_21      -0.0223444000
_diffrn_orient_matrix_UB_22      -0.0812869000
_diffrn_orient_matrix_UB_23      0.0057389000
_diffrn_orient_matrix_UB_31      -0.0836245000
_diffrn_orient_matrix_UB_32      0.0242472000
_diffrn_orient_matrix_UB_33      0.0012030000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0731
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            6224
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         31.995
_diffrn_reflns_theta_min         2.813
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.3048
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.0399
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 948 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.043(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0206P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.597
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.861
_reflns_number_gt                2986
_reflns_number_total             3289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00890f2.cif
_cod_data_source_block           rnp1405a
_cod_depositor_comments
'Adding full bibliography for 1549107--1549121.cif.'
_cod_original_cell_volume        2091.61(11)
_cod_database_code               1549110
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C18 H30 F4 Ni1 P2'
_chemical_oxdiff_usercomment     'Vargini Ni(f)(PEt3)2(C6F4I)'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_date_sample_data_collection 2014-01-31
_olex2_date_sample_submission    1386374400
_olex2_exptl_crystal_mounting_method 'Oil on loop.'
_olex2_submission_special_instructions 'No special instructions were received'