The Contrasting Character of Early and Late Transition Metal Fluorides as Hydrogen Bond Acceptors.
Smith, Dan A.; Beweries, Torsten; Blasius, Clemens; Jasim, Naseralla; Nazir, Ruqia; Nazir, Sadia; Robertson, Craig C.; Whitwood, Adrian C.; Hunter, Christopher A.; Brammer, Lee; Perutz, Robin N.; Journal of the American Chemical Society 137 (2015) 11820–11831; doi:10.1021/jacs.5b07509

data_4129521
_publ_section_title
;
 The Contrasting Character of Early and Late Transition Metal Fluorides as
 Hydrogen Bond Acceptors.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11820
_journal_page_last               11831
_journal_paper_doi               10.1021/jacs.5b07509
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C17 H32 F4 N2 Ni P2'
_chemical_formula_sum            'C17 H32 F4 N2 Ni P2'
_chemical_formula_weight         461.10
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-11-22
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.614(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0474(5)
_cell_length_b                   9.60545(18)
_cell_length_c                   16.7082(5)
_cell_measurement_reflns_used    11214
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      32.1078
_cell_measurement_theta_min      2.9270
_cell_volume                     2229.28(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
Palatinus, L. & Chapuis, G. (2007).
SUPERFLIP - a computer program for the solution of crystal structures
 by charge flipping in arbitrary dimensions.
J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
  1 omega  -67.00  -39.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1392 -178.0000    0.0000 28

  2 omega   -3.00   92.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455   77.0000  -90.0000 95

  3 omega   18.00   66.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455  -99.0000   90.0000 48

  4 omega  -25.00   53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455  -19.0000  120.0000 78

  5 omega -101.00  -35.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1392 -178.0000 -150.0000 66

  6 omega  -51.00   47.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1392   37.0000   60.0000 98

  7 omega    5.00   30.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455   57.0000   30.0000 25

  8 omega    1.00   99.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       26.5455   37.0000  150.0000 98
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0103557000
_diffrn_orient_matrix_UB_12      -0.0682527000
_diffrn_orient_matrix_UB_13      -0.0100758000
_diffrn_orient_matrix_UB_21      -0.0258761000
_diffrn_orient_matrix_UB_22      -0.0281776000
_diffrn_orient_matrix_UB_23      0.0239137000
_diffrn_orient_matrix_UB_31      -0.0427720000
_diffrn_orient_matrix_UB_32      0.0004036000
_diffrn_orient_matrix_UB_33      -0.0379589000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28647
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         32.18
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.050
_exptl_absorpt_correction_T_max  0.877
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
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)
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.5521
_exptl_crystal_size_mid          0.2569
_exptl_crystal_size_min          0.1292
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         7276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+1.6827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0960
_reflns_number_gt                5862
_reflns_number_total             7276
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b07509_si_002.cif
_cod_data_source_block           rnp1121
_cod_original_cell_volume        2229.27(13)
_cod_database_code               4129521