Coordinative trapping of the boron β-diketiminato system [B(NMesCMe)2CH] via metal-templated synthesis
Firinci, Erkan; Bates, Joshua I.; Riddlestone, Ian M.; Phillips, Nicholas; Aldridge, Simon; Chemical Communications (Cambridge, United Kingdom) 49 (2013) 1509–1511; doi:10.1039/c3cc38073d

data_7112333
_publ_section_title
;
 Coordinative trapping of the boron \b-diketiminato system
 [B(NMesCMe)2CH] via metal-templated synthesis
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   15
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1509
_journal_page_last               1511
_journal_paper_doi               10.1039/c3cc38073d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C25 H34 B1 Cl1 Fe1 N2 O2'
_chemical_formula_sum            'C25 H34 B Cl Fe N2 O2'
_chemical_formula_weight         496.67
_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
_cell_angle_alpha                90
_cell_angle_beta                 92.9406(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.30600(10)
_cell_length_b                   15.6594(2)
_cell_length_c                   13.3532(2)
_cell_measurement_reflns_used    6025
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2569.83(5)
_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 0.993
_diffrn_measured_fraction_theta_max 0.992
_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  0.027
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48165
_diffrn_reflns_theta_full        26.959
_diffrn_reflns_theta_max         27.510
_diffrn_reflns_theta_min         5.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_T_max  0.94
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.56
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9190
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5857
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0008378
_refine_ls_shift/su_mean         0.0000396
_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:
13.8 20.2 9.89 2.56
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1039
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.1039
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4379
_reflns_number_total             5857
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.29
_oxford_diffrn_Wilson_scale      12.04
_oxford_refine_ls_r_factor_ref   0.0577
_oxford_refine_ls_scale          0.2859(2)
_oxford_reflns_number_all        5857
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_duplicate_entry             7108846
_cod_data_source_file            c3cc38073d.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C25 H34 B1 Cl1 Fe1 N2 O2'
_cod_database_code               7112333
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) H ( 73,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) H ( 93,X'S)
RIDE C ( 10,X'S) H ( 103,X'S) H ( 102,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) H ( 203,X'S)
RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S) H ( 252,X'S) H ( 253,X'S)
RIDE C ( 26,X'S) H ( 263,X'S) H ( 262,X'S) H ( 261,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;