#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:09:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179278 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/98/4319881.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_4319881
loop_
_publ_author_name
'Tim J. Brunker'
'Tony Hascall'
'Andrew R. Cowley'
'Leigh H. Rees'
'Dermot O'Hare'
_publ_contact_author
;
Prof. Dermot O'Hare
Inorganic Chemistry Laboratory
University of Oxford
South Parks Rd.
Oxford
OX1 3QR
;
_publ_contact_author_email       'dermot.ohare@chem.ox.ac.uk '
_publ_contact_author_fax         ' +44 1865 272 690 '
_publ_contact_author_phone       ' +44 1865 272 658 '
_publ_section_title
;
 Variable Coordination Modes of
 Hydrotris(3-isopropyl-4-bromopyrazolyl)borate (Tp') in Fe(II), Mn(II),
 Cr(II), and Cr(III) Complexes: Formation of MTp'Cl (M = Fe and Mn),
 Structural Isomerism in CrTp'2, and the Observation of Tp'- as an
 Uncoordinated Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3170
_journal_page_last               3176
_journal_paper_doi               10.1021/ic010125k
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C18 H25 B1 Br3 Cl1 Mn1 N6'
_chemical_formula_structural     'C18 H25 BR3 B1 CL1 MN1 N6'
_chemical_formula_sum            'C18 H25 B Br3 Cl Mn N6'
_chemical_formula_weight         666.37
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      36
_symmetry_space_group_name_Hall  'C 2c -2c'
_symmetry_space_group_name_H-M   'C c m 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta3
_audit_creation_date             1999-10-01T13:58:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7810(4)
_cell_length_b                   14.3140(5)
_cell_length_c                   15.7680(4)
_cell_measurement_reflns_used    109
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     2433.31(14)
_computing_cell_refinement       DENZO
_computing_data_collection       'Enraf-Nonius DIP2000 Software - XPRESS'
_computing_data_reduction        'DENZO & SCALEPACK'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1365
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    5.596
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.53(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_gt    1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1365
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+2.1863P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.049
_refine_ls_wR_factor_gt          0.0484
_reflns_number_gt                1321
_reflns_number_total             1365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010125k_3.cif
_cod_data_source_block           str36c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.1863P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.1863P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319881
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, z+1/2'
'x, -y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Mn1 Mn 0.49303(8) 0 0.47581(6) 0.01423(15) Uani 1 d S .
Cl1 Cl 0.62799(11) 0 0.36511(10) 0.0209(2) Uani 1 d S .
B1 B 0.3121(5) 0 0.6264(3) 0.0142(10) Uani 1 d S .
H1 H 0.2539(5) 0 0.6741(3) 0.017 Uiso 1 calc SR .
Br1 Br -0.06243(4) 0 0.39583(4) 0.02017(12) Uani 1 d S .
Br2 Br 0.52775(4) 0.32474(2) 0.72903(3) 0.02710(11) Uani 1 d . .
N11 N 0.2963(4) 0 0.4649(3) 0.0181(8) Uani 1 d S .
C12 C 0.2081(4) 0 0.4052(4) 0.0173(10) Uani 1 d S .
C13 C 0.2377(5) 0 0.3125(4) 0.0214(10) Uani 1 d S .
H13 H 0.1587(5) 0 0.2817(4) 0.026 Uiso 1 calc SR .
C14 C 0.3081(4) -0.0879(3) 0.2865(3) 0.0311(9) Uani 1 d . .
H14A H 0.326(3) -0.0852(11) 0.2270(5) 0.047 Uiso 1 calc R .
H14B H 0.2580(13) -0.1419(3) 0.298(2) 0.047 Uiso 1 calc R .
H14C H 0.3840(15) -0.0918(13) 0.3181(16) 0.047 Uiso 1 calc R .
C15 C 0.0934(5) 0 0.4451(3) 0.0164(9) Uani 1 d S .
C16 C 0.1173(5) 0 0.5303(4) 0.0185(10) Uani 1 d S .
H16 H 0.0580(5) 0 0.5731(4) 0.022 Uiso 1 calc SR .
N17 N 0.2391(4) 0 0.5417(3) 0.0153(8) Uani 1 d S .
N21 N 0.4818(3) 0.1061(2) 0.5704(2) 0.0182(6) Uani 1 d . .
C22 C 0.5378(4) 0.1863(3) 0.5929(3) 0.0192(7) Uani 1 d . .
C23 C 0.6414(4) 0.2284(3) 0.5419(3) 0.0294(9) Uani 1 d . .
H23 H 0.6649(4) 0.2873(3) 0.5691(3) 0.035 Uiso 1 calc R .
C24 C 0.6005(5) 0.2507(3) 0.4515(3) 0.0366(10) Uani 1 d . .
H24A H 0.574(3) 0.1943(5) 0.4238(8) 0.055 Uiso 1 calc R .
H24B H 0.6686(11) 0.278(2) 0.4208(7) 0.055 Uiso 1 calc R .
H24C H 0.533(2) 0.294(2) 0.4529(3) 0.055 Uiso 1 calc R .
C25 C 0.7552(4) 0.1645(4) 0.5427(3) 0.0378(11) Uani 1 d . .
H25A H 0.8223(11) 0.1945(12) 0.513(2) 0.057 Uiso 1 calc R .
H25B H 0.7355(11) 0.1067(11) 0.515(2) 0.057 Uiso 1 calc R .
H25C H 0.779(2) 0.152(2) 0.6003(3) 0.057 Uiso 1 calc R .
C26 C 0.4845(3) 0.2179(2) 0.6669(2) 0.0174(7) Uani 1 d . .
C27 C 0.3947(3) 0.1551(2) 0.6888(2) 0.0177(7) Uani 1 d . .
H27 H 0.3432(3) 0.1585(2) 0.7360(2) 0.021 Uiso 1 calc R .
N28 N 0.3941(3) 0.0879(2) 0.6303(2) 0.0153(6) Uani 1 d . .
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 0 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
N11 Mn1 N21 90.02(11) . 4 ?
N11 Mn1 N21 90.02(11) . . ?
N21 Mn1 N21 90.9(2) 4 . ?
N11 Mn1 Cl1 125.16(13) . . ?
N21 Mn1 Cl1 124.98(8) 4 . ?
N21 Mn1 Cl1 124.99(8) . . ?
N28 B1 N28 109.7(4) 4 . ?
N28 B1 N17 109.0(3) 4 . ?
N28 B1 N17 109.0(3) . . ?
C12 N11 N17 107.7(4) . . ?
C12 N11 Mn1 140.0(4) . . ?
N17 N11 Mn1 112.3(3) . . ?
N11 C12 C15 108.4(5) . . ?
N11 C12 C13 122.3(5) . . ?
C15 C12 C13 129.3(5) . . ?
C12 C13 C14 111.6(3) . 4 ?
C12 C13 C14 111.6(3) . . ?
C14 C13 C14 111.1(5) 4 . ?
C16 C15 C12 106.1(4) . . ?
C16 C15 Br1 125.7(4) . . ?
C12 C15 Br1 128.2(4) . . ?
N17 C16 C15 108.7(5) . . ?
C16 N17 N11 109.2(4) . . ?
C16 N17 B1 128.3(4) . . ?
N11 N17 B1 122.5(4) . . ?
C22 N21 N28 107.0(3) . . ?
C22 N21 Mn1 140.2(3) . . ?
N28 N21 Mn1 112.8(2) . . ?
N21 C22 C26 108.5(3) . . ?
N21 C22 C23 122.3(3) . . ?
C26 C22 C23 129.2(3) . . ?
C22 C23 C24 111.7(4) . . ?
C22 C23 C25 110.7(4) . . ?
C24 C23 C25 111.3(3) . . ?
C27 C26 C22 107.1(3) . . ?
C27 C26 Br2 125.6(3) . . ?
C22 C26 Br2 127.3(3) . . ?
N28 C27 C26 107.7(3) . . ?
C27 N28 N21 109.8(3) . . ?
C27 N28 B1 128.3(3) . . ?
N21 N28 B1 121.9(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 N11 2.128(5) . ?
Mn1 N21 2.132(3) 4 ?
Mn1 N21 2.132(3) . ?
Mn1 Cl1 2.272(2) . ?
B1 N28 1.539(4) 4 ?
B1 N28 1.539(4) . ?
B1 N17 1.550(6) . ?
Br1 C15 1.851(5) . ?
Br2 C26 1.876(4) . ?
N11 C12 1.338(7) . ?
N11 N17 1.359(6) . ?
C12 C15 1.387(7) . ?
C12 C13 1.497(8) . ?
C13 C14 1.525(5) 4 ?
C13 C14 1.525(5) . ?
C15 C16 1.368(8) . ?
C16 N17 1.325(7) . ?
N21 C22 1.344(5) . ?
N21 N28 1.362(4) . ?
C22 C26 1.376(5) . ?
C22 C23 1.502(5) . ?
C23 C24 1.527(7) . ?
C23 C25 1.530(7) . ?
C26 C27 1.366(5) . ?
C27 N28 1.332(5) . ?
