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_4125255
_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(C15 H10 F6 N2 O), C16 H36 N, F'
_chemical_formula_sum            'C46 H56 F13 N5 O2'
_chemical_formula_weight         957.96
_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   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2013-06-06
_audit_creation_method           CRYSTALS_ver_14.52
_cell_angle_alpha                90
_cell_angle_beta                 92.7108(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9971(2)
_cell_length_b                   17.0640(4)
_cell_length_c                   24.9997(6)
_cell_measurement_reflns_used    9370
_cell_measurement_temperature    150
_cell_measurement_theta_max      26
_cell_measurement_theta_min      5
_cell_volume                     4686.06(18)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.108
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47775
_diffrn_reflns_theta_full        25.039
_diffrn_reflns_theta_max         26.357
_diffrn_reflns_theta_min         5.127
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2000.000
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.34
_refine_diff_density_min         -0.97
_refine_ls_extinction_coef       330(40)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0193
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         5811
_refine_ls_number_restraints     336
_refine_ls_R_factor_all          0.1342
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.0001066
_refine_ls_shift/su_mean         0.0000100
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 4.81 5.89 1.50 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2353
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.2353
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              0
_reflns_number_gt                3416
_reflns_number_total             9446
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.57
_oxford_diffrn_Wilson_scale      117.25
_oxford_refine_ls_r_factor_ref   0.1342
_oxford_refine_ls_scale          0.12279(12)
_oxford_reflns_number_all        5811
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 018gwp12
_cod_data_source_file            ja6b07501_si_002.cif
_cod_data_source_block           2b
_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.

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_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               4125255
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE F(1,X'S,U'S) UNTIL C(117) 
CONT F(100,U[ISO],SIZE) UNTIL F(400) 
CONT EXTPARAM 
REM CONT F(100,U[ISO],SIZE,DECLINATION,AZIMUTH) UNTIL F(400) 
EQUIV F(19,OCC) F(20,OCC) F(21,OCC) F(100,OCC) 
WEIGHT -3 F(100,OCC) 
EQUIV F(39,OCC) F(40,OCC) F(41,OCC) F(200,OCC) 
WEIGHT -3 F(200,OCC) 
EQUIV F(59,OCC) F(60,OCC) F(61,OCC) F(300,OCC) 
WEIGHT -3 F(300,OCC) 
EQUIV F(79,OCC) F(80,OCC) F(81,OCC) F(400,OCC) 
WEIGHT -3 F(400,OCC) 
RIDE C   (  18,X'S) F   ( 100,X'S) 
RIDE C   (  38,X'S) F   ( 200,X'S) 
RIDE C   (  58,X'S) F   ( 300,X'S) 
RIDE C   (  78,X'S) F   ( 400,X'S) 
RIDE N   (  11,X'S) H   ( 111,X'S) 
RIDE N   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  33,X'S) H   ( 331,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE N   (  51,X'S) H   ( 511,X'S) 
RIDE N   (  71,X'S) H   ( 711,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) H   (1022,X'S) 
RIDE C   ( 103,X'S) H   (1032,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) H   (1042,X'S) 
RIDE C   ( 105,X'S) H   (1052,X'S) H   (1051,X'S) H   (1053,X'S) 
RIDE C   ( 106,X'S) H   (1062,X'S) H   (1061,X'S) 
RIDE C   ( 107,X'S) H   (1071,X'S) H   (1072,X'S) 
RIDE C   ( 108,X'S) H   (1082,X'S) H   (1081,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) H   (1093,X'S) H   (1092,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) H   (1102,X'S) 
RIDE C   ( 111,X'S) H   (1112,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) H   (1122,X'S) 
RIDE C   ( 113,X'S) H   (1131,X'S) H   (1132,X'S) H   (1133,X'S) 
RIDE C   ( 114,X'S) H   (1142,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) H   (1152,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) H   (1162,X'S) 
RIDE C   ( 117,X'S) H   (1173,X'S) H   (1172,X'S) H   (1171,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
SIMU  0.01   C(15)  C(18)  F(19)  F(20)  F(21) AND 
CONT  C(15)  C(18)  F(20)  F(21)  F(19) AND 
CONT  C(15)  C(18)  F(21)  F(19)  F(20) AND 
CONT  C(35)  C(38)  F(39)  F(40)  F(41) AND 
CONT  C(35)  C(38)  F(40)  F(41)  F(39) AND 
CONT  C(35)  C(38)  F(41)  F(39)  F(40) AND 
CONT  C(55)  C(58)  F(59)  F(60)  F(61) AND 
CONT  C(55)  C(58)  F(60)  F(61)  F(59) AND 
CONT  C(55)  C(58)  F(61)  F(59)  F(60) AND 
CONT  C(75)  C(78)  F(79)  F(80)  F(81) AND 
CONT  C(75)  C(78)  F(80)  F(81)  F(79) AND 
CONT  C(75)  C(78)  F(81)  F(79)  F(80) 
DELU  0.01   C(15)  C(18)  F(19)  F(20)  F(21) AND 
CONT  C(15)  C(18)  F(20)  F(21)  F(19) AND 
CONT  C(15)  C(18)  F(21)  F(19)  F(20) AND 
CONT  C(35)  C(38)  F(39)  F(40)  F(41) AND 
CONT  C(35)  C(38)  F(40)  F(41)  F(39) AND 
CONT  C(35)  C(38)  F(41)  F(39)  F(40) AND 
CONT  C(55)  C(58)  F(59)  F(60)  F(61) AND 
CONT  C(55)  C(58)  F(60)  F(61)  F(59) AND 
CONT  C(55)  C(58)  F(61)  F(59)  F(60) AND 
CONT  C(75)  C(78)  F(79)  F(80)  F(81) AND 
CONT  C(75)  C(78)  F(80)  F(81)  F(79) AND 
CONT  C(75)  C(78)  F(81)  F(79)  F(80) 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;