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_7108848
_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         'C32 H12 B F24, C35 H44 B Fe N2 O2'
_chemical_formula_sum            'C67 H56 B2 F24 Fe N2 O2'
_chemical_formula_weight         1454.61
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             12-07-13
_audit_creation_method           CRYSTALS_ver_14.23
_cell_angle_alpha                87.9149(9)
_cell_angle_beta                 87.6232(9)
_cell_angle_gamma                78.9774(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1918(3)
_cell_length_b                   16.3393(4)
_cell_length_c                   17.0192(5)
_cell_measurement_reflns_used    13511
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3323.51(15)
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.990
_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  0.036
_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       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50955
_diffrn_reflns_theta_full        25.171
_diffrn_reflns_theta_max         27.066
_diffrn_reflns_theta_min         5.121
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8912
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     995
_refine_ls_number_reflns         14457
_refine_ls_number_restraints     648
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.0096230
_refine_ls_shift/su_mean         0.0001931
_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:
18.5 26.1 11.8 2.71
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1827
_refine_ls_wR_factor_gt          0.1546
_refine_ls_wR_factor_ref         0.1827
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                10180
_reflns_number_total             14458
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.76
_oxford_diffrn_Wilson_scale      12.53
_oxford_refine_ls_r_factor_ref   0.1026
_oxford_refine_ls_scale          0.3242(3)
_oxford_reflns_number_all        14458
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 063efnp12
_cod_data_source_file            c3cc38073d.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct' changed to 'direct'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C67 H56 B2 F24 Fe1 N2 O2'
_cod_database_code               7108848
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
EQUIV PART(1001,OCC) PART(1002,OCC)
WEIGHT -1 PART(1002,OCC)
EQUIV PART(2001,OCC) PART(2002,OCC)
WEIGHT -1 PART(2002,OCC)
EQUIV PART(3001,OCC) PART(3002,OCC)
WEIGHT -1 PART(3002,OCC)
EQUIV PART(4001,OCC) PART(4002,OCC)
WEIGHT -1 PART(4002,OCC)
END
;
_iucr_refine_instruction_details_restraints
;
SAME C(77) F(300) F(301) F(302) AND
CONT C(77) F(301) F(302) F(300) AND
CONT C(77) F(302) F(300) F(301) AND
CONT C(77) F(303) F(304) F(305) AND
CONT C(77) F(304) F(305) F(303) AND
CONT C(77) F(305) F(303) F(304)
SIMU 0.01 C(77) F(300) F(301) F(302) AND
CONT C(77) F(301) F(302) F(300) AND
CONT C(77) F(302) F(300) F(301) AND
CONT C(77) F(303) F(304) F(305) AND
CONT C(77) F(304) F(305) F(303) AND
CONT C(77) F(305) F(303) F(304)
DELU 0.01 C(77) F(300) F(301) F(302) AND
CONT C(77) F(301) F(302) F(300) AND
CONT C(77) F(302) F(300) F(301) AND
CONT C(77) F(303) F(304) F(305) AND
CONT C(77) F(304) F(305) F(303) AND
CONT C(77) F(305) F(303) F(304)
SAME C(95) F(400) F(401) F(402) AND
CONT C(95) F(401) F(402) F(400) AND
CONT C(95) F(402) F(400) F(401) AND
CONT C(95) F(403) F(404) F(405) AND
CONT C(95) F(404) F(405) F(403) AND
CONT C(95) F(405) F(403) F(404)
SIMU 0.01 C(95) F(400) F(401) F(402) AND
CONT C(95) F(401) F(402) F(400) AND
CONT C(95) F(402) F(400) F(401) AND
CONT C(95) F(403) F(404) F(405) AND
CONT C(95) F(404) F(405) F(403) AND
CONT C(95) F(405) F(403) F(404)
DELU 0.01 C(95) F(400) F(401) F(402) AND
CONT C(95) F(401) F(402) F(400) AND
CONT C(95) F(402) F(400) F(401) AND
CONT C(95) F(403) F(404) F(405) AND
CONT C(95) F(404) F(405) F(403) AND
CONT C(95) F(405) F(403) F(404)
SAME C(81) F(500) F(501) F(502) AND
CONT C(81) F(501) F(502) F(500) AND
CONT C(81) F(502) F(500) F(501) AND
CONT C(81) F(503) F(504) F(505) AND
CONT C(81) F(504) F(505) F(503) AND
CONT C(81) F(505) F(503) F(504)
SIMU 0.01 C(81) F(500) F(501) F(502) AND
CONT C(81) F(501) F(502) F(500) AND
CONT C(81) F(502) F(500) F(501) AND
CONT C(81) F(503) F(504) F(505) AND
CONT C(81) F(504) F(505) F(503) AND
CONT C(81) F(505) F(503) F(504)
DELU 0.01 C(81) F(500) F(501) F(502) AND
CONT C(81) F(501) F(502) F(500) AND
CONT C(81) F(502) F(500) F(501) AND
CONT C(81) F(503) F(504) F(505) AND
CONT C(81) F(504) F(505) F(503) AND
CONT C(81) F(505) F(503) F(504)
SAME C(67) F(600) F(601) F(602) AND
CONT C(67) F(601) F(602) F(600) AND
CONT C(67) F(602) F(600) F(601) AND
CONT C(67) F(603) F(604) F(605) AND
CONT C(67) F(604) F(605) F(603) AND
CONT C(67) F(605) F(603) F(604)
SIMU 0.01 C(67) F(600) F(601) F(602) AND
CONT C(67) F(601) F(602) F(600) AND
CONT C(67) F(602) F(600) F(601) AND
CONT C(67) F(603) F(604) F(605) AND
CONT C(67) F(604) F(605) F(603) AND
CONT C(67) F(605) F(603) F(604)
DELU 0.01 C(67) F(600) F(601) F(602) AND
CONT C(67) F(601) F(602) F(600) AND
CONT C(67) F(602) F(600) F(601) AND
CONT C(67) F(603) F(604) F(605) AND
CONT C(67) F(604) F(605) F(603) AND
CONT C(67) F(605) F(603) F(604)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;