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_1549112
_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      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-16
_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            8
_cell_length_a                   14.0519(2)
_cell_length_b                   14.4485(3)
_cell_length_c                   24.3473(5)
_cell_measurement_reflns_used    6938
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      31.8480
_cell_measurement_theta_min      3.6290
_cell_volume                     4943.20(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00 100.00   1.00   30.00    --   25.48 178.00 150.00   65
  2  \w    -41.00  30.00   1.00   30.00    --   25.48 -57.00 -90.00   71
  3  \w     40.00  67.00   1.00   30.00    --   25.48 178.00  60.00   27
  4  \w    -85.00 -47.00   1.00   30.00    --  -26.10 -19.00 -30.00   38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0057575000
_diffrn_orient_matrix_UB_12      0.0488177000
_diffrn_orient_matrix_UB_13      0.0000128000
_diffrn_orient_matrix_UB_21      0.0440105000
_diffrn_orient_matrix_UB_22      -0.0048413000
_diffrn_orient_matrix_UB_23      -0.0140235000
_diffrn_orient_matrix_UB_31      -0.0240613000
_diffrn_orient_matrix_UB_32      0.0026582000
_diffrn_orient_matrix_UB_33      -0.0255031000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            21001
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.080
_diffrn_reflns_theta_min         3.331
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.444
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.325
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.873
_exptl_crystal_description       plate
_exptl_crystal_F_000             2704
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Chloroform'
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         7245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0149P)^2^+5.8182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5931
_reflns_number_total             7245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc00890f2.cif
_cod_data_source_block           1oI(beta)_rnp1538a
_cod_depositor_comments
'Adding full bibliography for 1549107--1549121.cif.'
_cod_original_cell_volume        4943.18(16)
_cod_database_code               1549112
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C18 H30 F4 I2 Ni1 P2'
_chemical_oxdiff_usercomment     'Sarah SP202 rpt'
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.431
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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(F3A) = Uanis(F1)
Uanis(F2A) = Uanis(F2)
Uanis(F3) = Uanis(F4A)
Uanis(C2A) = Uanis(C6)
Uanis(C5) = Uanis(C3A)
Uanis(C6A) = Uanis(C2)
Uanis(C5A) = Uanis(C3)
Uanis(C4) = Uanis(C4A)
Uanis(C1) = Uanis(C1A)
Uanis(I1) = Uanis(I1A)
Uanis(F1A) = Uanis(F3)
3. Others
 Sof(C1A)=Sof(C6A)=Sof(C5A)=Sof(C4A)=Sof(C3A)=Sof(C2A)=Sof(F1A)=Sof(F2A)=
 Sof(F3A)=Sof(F4A)=Sof(I1A)=Sof(I2A)=1-FVAR(1)
 Sof(C1)=Sof(C2)=Sof(C3)=Sof(C4)=Sof(C5)=Sof(C6)=Sof(F1)=Sof(F2)=Sof(F3)=
 Sof(F4)=Sof(I1)=Sof(I2)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B),
 C17(H17A,H17B)
4.b Fitted hexagon refined as free rotating group:
 C1A(C6A,C5A,C4A,C3A,C2A)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              29542
_shelx_hkl_checksum              22853
_olex2_date_sample_data_collection 2015-09-08
_olex2_date_sample_submission    2015-09-07
_olex2_exptl_crystal_mounting_method 'oil on loop'
_olex2_submission_original_sample_id SP202
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.770