Catalytic B-N Dehydrogenation Using Frustrated Lewis Pairs: Evidence for a Chain-Growth Coupling Mechanism.
Mo, Zhenbo; Rit, Arnab; Campos, Jesús; Kolychev, Eugene L.; Aldridge, Simon; Journal of the American Chemical Society 138 (2016) 3306–3309; doi:10.1021/jacs.6b01170

data_4130183
_publ_section_title
;
 Catalytic B-N Dehydrogenation Using Frustrated Lewis Pairs: Evidence for
 a Chain-Growth Coupling Mechanism.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3306
_journal_page_last               3309
_journal_paper_doi               10.1021/jacs.6b01170
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C39 H32 B3 F10 N2 O1 P1'
_chemical_formula_sum            'C39 H32 B3 F10 N2 O P'
_chemical_formula_weight         798.08
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 91.9390(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.97190(10)
_cell_length_b                   17.3317(2)
_cell_length_c                   21.4305(3)
_cell_measurement_reflns_used    8316
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3701.71(8)
_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 0.990
_diffrn_measured_fraction_theta_max 0.988
_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  0.031
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15744
_diffrn_reflns_theta_full        25.013
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         5.131
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.160
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.53
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9627
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         8380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.0008469
_refine_ls_shift/su_mean         0.0000334
_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: 
 15.1 20.9 9.83 2.42 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1137
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.1137
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                5843
_reflns_number_total             8380
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.57
_oxford_diffrn_Wilson_scale      3.96
_oxford_refine_ls_r_factor_ref   0.0778
_oxford_refine_ls_scale          0.3386(3)
_oxford_reflns_number_all        8380
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_iucr_refine_instructions_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (  21,X'S) H   (  21,X'S) 
RIDE C   (  20,X'S) H   (  20,X'S) 
RIDE C   (  19,X'S) H   (  19,X'S) 
RIDE C   (  18,X'S) H   (  18,X'S) 
RIDE C   (  17,X'S) H   (  17,X'S) 
RIDE C   (  23,X'S) H   (  23,X'S) 
RIDE C   (  24,X'S) H   (  24,X'S) 
RIDE C   (  25,X'S) H   (  25,X'S) 
RIDE C   (  26,X'S) H   (  26,X'S) 
RIDE C   (  27,X'S) H   (  27,X'S) 
RIDE C   (  13,X'S) H   (  13,X'S) 
RIDE C   (  12,X'S) H   (  12,X'S) 
RIDE C   (  11,X'S) H   (  11,X'S) 
RIDE C   (   4,X'S) H   (   4,X'S) 
RIDE C   (   3,X'S) H   (   3,X'S) 
RIDE C   (   2,X'S) H   (   2,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) H   (  93,X'S) H   (  92,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) H   (  82,X'S) H   (  83,X'S) 
RIDE B   (   1,X'S) H   (   1,X'S) 
RIDE B   (   2,X'S) H   ( 211,X'S) H   ( 212,X'S) 
RIDE N   (   1,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE B   (   3,X'S) H   ( 311,X'S) H   ( 312,X'S) 
RIDE N   (   2,X'S) H   ( 214,X'S) H   ( 215,X'S) H   ( 213,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
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_cod_data_source_file            ja6b01170_si_002.cif
_cod_data_source_block           2-HBH2NH2BH2NH3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C39 H32 B3 F10 N2 O1 P1'
_cod_database_code               4130183