Hydrogen-Bonded Homoleptic Fluoride-Diarylurea Complexes: Structure, Reactivity, and Coordinating Power.
Pfeifer, Lukas; Engle, Keary M.; Pidgeon, George W.; Sparkes, Hazel A.; Thompson, Amber L.; Brown, John M.; Gouverneur, Véronique; Journal of the American Chemical Society 138 (2016) 13314–; doi:10.1021/jacs.6b07501

data_4125278
_publ_section_title
;
 Hydrogen-Bonded Homoleptic Fluoride-Diarylurea Complexes: Structure,
 Reactivity, and Coordinating Power.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13314
_journal_paper_doi               10.1021/jacs.6b07501
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         '2(C13 H10 F2 N2 O), C16 H36 N, F'
_chemical_formula_sum            'C42 H56 F5 N5 O2'
_chemical_formula_weight         757.93
_chemical_melting_point          ?
_space_group_IT_number           14
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.209(4)
_cell_length_b                   14.686(6)
_cell_length_c                   21.024(8)
_cell_measurement_reflns_used    330
_cell_measurement_temperature    150(2)
_cell_volume                     4055(3)
_computing_cell_refinement       'SXD2001 (Gutmann, 2005)'
_computing_data_collection       'SXD2001 (Gutmann, 2005)'
_computing_data_reduction        'SXD2001 (Gutmann, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.041
_diffrn_measured_fraction_theta_max 0.041
_diffrn_measurement_device_type  'SXD at ISIS neutron source'
_diffrn_measurement_method       'time-of-flight Laue diffraction'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'ISIS spallation neutron source'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     Laue
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0481
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -80
_diffrn_reflns_number            10529
_diffrn_reflns_theta_full        83.90
_diffrn_reflns_theta_max         83.90
_diffrn_reflns_theta_min         8.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Crystal size used:  Spherical, radius 3 mm
Mu: (4.8722 + 0.0156 * lambda) cm^-1^
;
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             626
_exptl_crystal_size_max          10.0
_exptl_crystal_size_mid          9.0
_exptl_crystal_size_min          8.0
_refine_diff_density_max         1.766
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.318
_refine_ls_extinction_coef       0.00131(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.319
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     998
_refine_ls_number_reflns         10529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.319
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.1031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2639
_refine_ls_wR_factor_ref         0.2639
_reflns_number_gt                10529
_reflns_number_total             10529
_reflns_threshold_expression     >2sigma(I)
_oxford_structure_analysis_title 019gwp12/Neutron5
_cod_data_source_file            ja6b07501_si_002.cif
_cod_data_source_block           2j-neutron
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 4125254--4125278.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               4125278