Energetics of Halogen Bonding of Group 10 Metal Fluoride Complexes
Torsten Beweries; Lee Brammer; Naseralla A. Jasim; John E. McGrady; Robin N. Perutz; Adrian C. Whitwood; Journal of the American Chemical Society 133 (2011) 14338–14348; doi:10.1021/ja203320y

data_4106744
_publ_contact_author_address
;Department of Chemistry,
University of York,
Heslington,
York, YO10 5DD
UK
;
_publ_contact_author_email       robin.perutz@york.ac.uk
_publ_contact_author_name        'Professor Robin N. Perutz'
_publ_section_title
;
 Energetics of Halogen Bonding of Group 10 Metal Fluoride Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14338
_journal_page_last               14348
_journal_paper_doi               10.1021/ja203320y
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C36 H55 F6 N Ni P2'
_chemical_formula_sum            'C36 H55 F6 N Ni P2'
_chemical_formula_weight         736.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.3446(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5066(3)
_cell_length_b                   12.3458(2)
_cell_length_c                   19.7390(3)
_cell_measurement_reflns_used    8067
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      29.9978
_cell_measurement_theta_min      3.0095
_cell_volume                     3534.19(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'smtbx-flip (Bourhis, 2008)'
_diffrn_ambient_temperature      110.0
_diffrn_detector_area_resol_mean 16.145
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
1 omega  -51.00    1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
-      -24.9830  -37.0000  -30.0000 52

2 omega    5.00   97.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
-       26.3892   37.0000  -90.0000 92

3 omega  -43.00   48.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
-       26.3892  -37.0000   90.0000 91
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0407387
_diffrn_orient_matrix_UB_12      0.023483
_diffrn_orient_matrix_UB_13      0.0127119
_diffrn_orient_matrix_UB_21      0.0269435
_diffrn_orient_matrix_UB_22      0.031712
_diffrn_orient_matrix_UB_23      0.0229655
_diffrn_orient_matrix_UB_31      0.0023845
_diffrn_orient_matrix_UB_32      0.041716
_diffrn_orient_matrix_UB_33      -0.0245923
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19381
_diffrn_reflns_theta_full        30.06
_diffrn_reflns_theta_max         30.06
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.9938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.1673
_exptl_crystal_size_min          0.1443
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         10333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+1.8934P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0917
_reflns_number_gt                8174
_reflns_number_total             10333
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja203320y_si_001_1.cif
_cod_data_source_block           RNP1023
_cod_original_cell_volume        3534.18(12)
_cod_database_code               4106744