#------------------------------------------------------------------------------
#$Date: 2016-10-08 01:10:15 +0300 (Sat, 08 Oct 2016) $
#$Revision: 187092 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/04/7040401.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7040401
loop_
_publ_author_name
'Antiñolo, Antonio'
'Carrillo-Hermosilla, Fernando'
'Fernández-Galán, Rafael'
'Montero-Rama, María Pilar'
'Ramos, Alberto'
'Villaseñor, Elena'
'Rojas, Rene S.'
'Rodríguez-Diéguez, Antonio'
_publ_section_title
;
 Dialkylboron guanidinates: syntheses, structures and carbodiimide
 de-insertion reactions.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15350
_journal_paper_doi               10.1039/c6dt02913b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C23 H42 B N3'
_chemical_formula_weight         371.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-05-13 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.655(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9050(19)
_cell_length_b                   20.244(3)
_cell_length_c                   10.069(2)
_cell_measurement_reflns_used    5459
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.85
_cell_volume                     2222.7(7)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker ApexII'
_computing_data_reduction        'Bruker Apex II'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'Phi and Omega Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.723
_diffrn_reflns_theta_min         2.853
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.676
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1555
_refine_ls_R_factor_gt           0.1174
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1387P)²+17.0679P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2958
_refine_ls_wR_factor_ref         0.3235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2069
_reflns_number_total             2892
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02913b2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

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

 Adding full bibliography for 7040401--7040404.cif.
;
_cod_original_cell_volume        2222.5(7)
_cod_database_code               7040401
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
B1 B 0.0000 0.1274(2) 0.7500 0.0141(9) Uani 1 2 d S T P
C1 C 0.0000 0.2297(2) 0.7500 0.0163(9) Uani 1 2 d S T P
C2 C 0.0499(3) 0.20491(17) 0.9880(3) 0.0207(7) Uani 1 1 d . . .
H2 H 0.1188 0.2355 0.9998 0.025 Uiso 1 1 calc R U .
C3 C 0.0779(3) 0.14311(18) 1.0687(3) 0.0244(8) Uani 1 1 d . . .
H3A H 0.0110 0.1126 1.0601 0.037 Uiso 1 1 calc R U .
H3B H 0.0889 0.1548 1.1605 0.037 Uiso 1 1 calc R U .
H3C H 0.1515 0.1229 1.0366 0.037 Uiso 1 1 calc R U .
C4 C -0.0650(5) 0.2384(2) 1.0426(4) 0.0408(11) Uani 1 1 d . . .
H4A H -0.0900 0.2734 0.9839 0.061 Uiso 1 1 calc R U .
H4B H -0.0470 0.2563 1.1290 0.061 Uiso 1 1 calc R U .
H4C H -0.1298 0.2066 1.0492 0.061 Uiso 1 1 calc R U .
C5 C 0.0974(5) 0.33418(19) 0.8146(4) 0.0373(10) Uani 1 1 d . . .
H5A H 0.0680 0.3523 0.8963 0.056 Uiso 1 1 calc R U .
H5B H 0.1231 0.3694 0.7573 0.056 Uiso 1 1 calc R U .
H5C H 0.1656 0.3055 0.8328 0.056 Uiso 1 1 calc R U .
C6 C -0.2320(3) 0.12192(18) 0.8387(5) 0.0352(10) Uani 1 1 d . . .
H6 H -0.2220 0.1692 0.8564 0.042 Uiso 1 1 calc R U .
C7 C -0.3023(4) 0.0845(2) 0.9417(5) 0.0363(10) Uani 1 1 d . . .
H7A H -0.3739 0.1091 0.9696 0.044 Uiso 1 1 calc R U .
H7B H -0.2512 0.0751 1.0189 0.044 Uiso 1 1 calc R U .
C8 C -0.3401(3) 0.01961(18) 0.8685(4) 0.0265(8) Uani 1 1 d . . .
H8A H -0.2999 -0.0184 0.9084 0.032 Uiso 1 1 calc R U .
H8B H -0.4281 0.0132 0.8712 0.032 Uiso 1 1 calc R U .
C9 C -0.2975(4) 0.0299(2) 0.7263(5) 0.0375(10) Uani 1 1 d . . .
H9 H -0.3409 0.0028 0.6603 0.045 Uiso 1 1 calc R U .
C10 C -0.1608(4) 0.0261(2) 0.7188(4) 0.0347(10) Uani 1 1 d . . .
H10A H -0.1339 0.0311 0.6278 0.042 Uiso 1 1 calc R U .
H10B H -0.1313 -0.0160 0.7527 0.042 Uiso 1 1 calc R U .
C11 C -0.1125(3) 0.08460(15) 0.8074(3) 0.0147(6) Uani 1 1 d . . .
H11 H -0.0835 0.0651 0.8911 0.018 Uiso 1 1 calc R U .
C12 C -0.3120(3) 0.1040(2) 0.7055(5) 0.0321(9) Uani 1 1 d . . .
H12A H -0.3965 0.1187 0.7101 0.039 Uiso 1 1 calc R U .
H12B H -0.2745 0.1196 0.6244 0.039 Uiso 1 1 calc R U .
N1 N 0.0398(2) 0.18887(12) 0.8457(3) 0.0141(6) Uani 1 1 d . . .
N2 N 0.0000 0.29696(19) 0.7500 0.0266(10) Uani 1 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C11 B1 C11 115.1(4) 2_556 .
C11 B1 N1 115.03(15) 2_556 .
C11 B1 N1 113.36(16) . .
C11 B1 N1 113.36(16) 2_556 2_556
C11 B1 N1 115.03(15) . 2_556
N1 B1 N1 80.4(3) . 2_556
C11 B1 C1 122.45(18) 2_556 .
C11 B1 C1 122.45(18) . .
N1 B1 C1 40.21(14) . .
N1 B1 C1 40.21(14) 2_556 .
N1 C1 N1 103.8(4) 2_556 .
N1 C1 N2 128.12(18) 2_556 .
N1 C1 N2 128.12(18) . .
N1 C1 B1 51.88(18) 2_556 .
N1 C1 B1 51.88(18) . .
N2 C1 B1 180.0 . .
N1 C2 C3 110.5(3) . .
N1 C2 C4 113.3(3) . .
C3 C2 C4 109.4(3) . .
C7 C6 C11 109.5(3) . .
C7 C6 C12 100.5(3) . .
C11 C6 C12 99.7(3) . .
C6 C7 C8 103.4(3) . .
C9 C8 C7 104.3(3) . .
C10 C9 C8 110.8(4) . .
C10 C9 C12 98.4(3) . .
C8 C9 C12 103.4(4) . .
C9 C10 C11 105.0(3) . .
C6 C11 C10 101.9(3) . .
C6 C11 B1 117.2(3) . .
C10 C11 B1 116.9(3) . .
C9 C12 C6 93.0(3) . .
C1 N1 C2 125.8(3) . .
C1 N1 B1 87.9(2) . .
C2 N1 B1 139.5(2) . .
C1 N2 C5 121.3(2) . 2_556
C1 N2 C5 121.3(2) . .
C5 N2 C5 117.4(4) 2_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
B1 C11 1.614(4) 2_556
B1 C11 1.614(4) .
B1 N1 1.630(4) .
B1 N1 1.630(4) 2_556
B1 C1 2.071(6) .
C1 N1 1.338(4) 2_556
C1 N1 1.338(4) .
C1 N2 1.362(6) .
C2 N1 1.472(4) .
C2 C3 1.521(5) .
C2 C4 1.532(5) .
C5 N2 1.450(4) .
C6 C7 1.502(6) .
C6 C11 1.542(4) .
C6 C12 1.632(7) .
C7 C8 1.559(6) .
C8 C9 1.525(6) .
C9 C10 1.496(6) .
C9 C12 1.522(6) .
C10 C11 1.571(5) .
N2 C5 1.450(4) 2_556
