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_1549121
_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 I2 Ni P2'
_chemical_formula_sum            'C18 H30 F4 I2 Ni P2'
_chemical_formula_weight         696.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-11-26
_audit_creation_method
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Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
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_audit_update_record
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2018-02-23 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6129(13)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.19004(19)
_cell_length_b                   28.0191(5)
_cell_length_c                   14.2344(2)
_cell_measurement_reflns_used    8425
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      70.5970
_cell_measurement_theta_min      3.4820
_cell_volume                     4859.89(13)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -15.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 77

  2 omega    8.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000  150.0000 64

  3 omega    8.00   95.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   90.0000 87

  4 omega   -2.00   70.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000  -60.0000 72

  5 omega   38.00   65.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 27

  6 omega   24.00  123.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000 -150.0000 99

  7 omega   86.00  111.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 25

  8 omega   40.00   99.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   60.0000 59

  9 omega   75.00  114.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 39

 10 omega   37.00   89.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -37.0000  120.0000 52

 11 omega   36.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 34

 12 omega   39.00  103.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -90.0000 64

 13 omega   55.00   91.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   60.0000 36

 14 omega   37.00   92.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 55

 15 omega   47.00   94.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -150.0000 47

 16 omega   36.00  145.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000   60.0000 109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0258855000
_diffrn_orient_matrix_UB_12      -0.0232643000
_diffrn_orient_matrix_UB_13      0.0961673000
_diffrn_orient_matrix_UB_21      -0.0913078000
_diffrn_orient_matrix_UB_22      0.0298409000
_diffrn_orient_matrix_UB_23      0.0441746000
_diffrn_orient_matrix_UB_31      -0.0834217000
_diffrn_orient_matrix_UB_32      -0.0399014000
_diffrn_orient_matrix_UB_33      -0.0230910000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18154
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.076
_diffrn_reflns_theta_max         67.076
_diffrn_reflns_theta_min         3.484
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.643
_exptl_absorpt_correction_T_max  0.576
_exptl_absorpt_correction_T_min  0.157
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       plate
_exptl_crystal_F_000             2704
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform'
_exptl_crystal_size_max          0.1492
_exptl_crystal_size_mid          0.0859
_exptl_crystal_size_min          0.0384
_refine_diff_density_max         1.241
_refine_diff_density_min         -0.910
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         8677
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0452P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7565
_reflns_number_total             8677
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00890f2.cif
_cod_data_source_block           1oI(gamma)_rnp1539
_cod_depositor_comments
'Adding full bibliography for 1549107--1549121.cif.'
_cod_original_cell_volume        4859.88(13)
_cod_database_code               1549121
_chemical_oxdiff_formula         'C18 H30 F4 I2 Ni1 P2'
_chemical_oxdiff_usercomment     'Sarah SP202 crystals at base'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C7B(H7BA,H7BB), C9B(H9BA,H9BB), C11B(H11A,H11B), C13B(H13A,H13B), C15B(H15A,
 H15B), C17B(H17A,H17B), C7A(H7AA,H7AB), C9A(H9AA,H9AB), C11A(H11C,H11D),
 C13A(H13C,H13D), C15A(H15C,H15D), C17A(H17C,H17D)
2.b Idealised Me refined as rotating group:
 C8B(H8BA,H8BB,H8BC), C10B(H10A,H10B,H10C), C12B(H12A,H12B,H12C), C14B(H14A,
 H14B,H14C), C16B(H16A,H16B,H16C), C18B(H18A,H18B,H18C), C8A(H8AA,H8AB,H8AC),
 C10A(H10D,H10E,H10F), C12A(H12D,H12E,H12F), C14A(H14D,H14E,H14F), C16A(H16D,
 H16E,H16F), C18A(H18D,H18E,H18F)
;
_shelx_res_checksum              3207
_shelx_hkl_checksum              89325
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-09-08
_olex2_date_sample_submission    2015-09-07
_olex2_submission_original_sample_id 'Sarah SP202'
_olex2_submission_special_instructions 'No special instructions were received'