#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/27/7012738.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_7012738
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Lee, Ting Huei'
'Leigh, G. Jeffery'
_publ_section_title
;
 The synthesis and properties of a new linear NPN proligand
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2276
_journal_paper_doi               10.1039/b300596h
_journal_year                    2003
_chemical_formula_sum            'C20 H40 Br6 Ni3 O5'
_chemical_formula_weight         1016.11
_chemical_name_common            '[Ni3Br6(thf)5]'
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_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_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2001-02-13T09:57:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.690(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5876(11)
_cell_length_b                   21.728(3)
_cell_length_c                   9.1261(12)
_cell_measurement_reflns_used    55160
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.967
_cell_measurement_theta_min      3.705
_cell_volume                     1502.9(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0805
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4980
_diffrn_reflns_theta_full        21.93
_diffrn_reflns_theta_max         21.93
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    9.865
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.243
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998)
I/sigma threshold for reflections     =   5.000
Delta(U)/lambda**2                    =   0.000
Highest even order spherical harmonic =       6
Highest odd  order spherical harmonic =       3
;
_exptl_crystal_density_diffrn    2.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.68
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         1809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0698
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0819P)²+20.5544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1893
_reflns_number_gt                1357
_reflns_number_total             1809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300596h.txt
_cod_data_source_block           feb1801
_cod_original_cell_volume        1502.9(3)
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               7012738
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_factor_mur        0.926
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.0141(3) 0.41664(8) 0.9638(2) 0.0268(6) Uani 1 1 d . . .
Ni2 Ni 0.0538(4) 0.25 0.8981(3) 0.0307(8) Uani 1 2 d S . .
Br1 Br -0.1870(2) 0.50396(7) 0.88072(16) 0.0307(5) Uani 1 1 d . . .
Br2 Br -0.1556(2) 0.33302(7) 0.81060(17) 0.0323(5) Uani 1 1 d . . .
Br3 Br 0.2144(2) 0.32932(7) 1.04762(18) 0.0366(6) Uani 1 1 d . . .
O1 O 0.1758(13) 0.4323(5) 0.7859(10) 0.033(3) Uani 1 1 d . . .
O2 O -0.1495(13) 0.3983(5) 1.1414(10) 0.034(3) Uani 1 1 d . . .
O3 O 0.205(2) 0.25 0.7233(16) 0.047(4) Uani 1 2 d S . .
C1 C 0.108(3) 0.4378(10) 0.6364(17) 0.052(5) Uani 1 1 d . . .
H1A H 0.0315 0.4744 0.625 0.062 Uiso 1 1 calc R . .
H1B H 0.0388 0.4009 0.6073 0.062 Uiso 1 1 calc R . .
C2 C 0.263(3) 0.4439(10) 0.5444(19) 0.058(6) Uani 1 1 d . . .
H2A H 0.2548 0.4822 0.4858 0.069 Uiso 1 1 calc R . .
H2B H 0.2696 0.4085 0.4765 0.069 Uiso 1 1 calc R . .
C3 C 0.423(2) 0.4455(10) 0.6463(17) 0.054(5) Uani 1 1 d . . .
H3A H 0.5064 0.4128 0.6201 0.065 Uiso 1 1 calc R . .
H3B H 0.4831 0.4858 0.639 0.065 Uiso 1 1 calc R . .
C4 C 0.367(3) 0.4362(10) 0.7948(19) 0.056(5) Uani 1 1 d . . .
H4A H 0.4182 0.3977 0.8363 0.068 Uiso 1 1 calc R . .
H4B H 0.4057 0.471 0.8584 0.068 Uiso 1 1 calc R . .
C5 C -0.338(2) 0.3848(10) 1.1316(18) 0.055(5) Uani 1 1 d . . .
H5A H -0.362 0.3514 1.0596 0.066 Uiso 1 1 calc R . .
H5B H -0.4041 0.4217 1.0971 0.066 Uiso 1 1 calc R . .
C6 C -0.399(3) 0.3659(12) 1.276(2) 0.075(7) Uani 1 1 d . . .
H6A H -0.4626 0.3262 1.2693 0.09 Uiso 1 1 calc R . .
H6B H -0.4773 0.3974 1.3164 0.09 Uiso 1 1 calc R . .
C7 C -0.227(3) 0.3599(17) 1.370(3) 0.130(14) Uani 1 1 d . . .
H7A H -0.232 0.3856 1.4594 0.156 Uiso 1 1 calc R . .
H7B H -0.2076 0.3166 1.4004 0.156 Uiso 1 1 calc R . .
C8 C -0.087(3) 0.3801(10) 1.2830(18) 0.056(6) Uani 1 1 d . . .
H8A H -0.0254 0.4152 1.3322 0.067 Uiso 1 1 calc R . .
H8B H -0.0002 0.3464 1.2744 0.067 Uiso 1 1 calc R . .
C9 C 0.140(4) 0.25 0.575(2) 0.053(7) Uani 1 2 d S . .
H9A H 0.067 0.287 0.555 0.063 Uiso 0.5 1 calc PR . .
H9B H 0.067 0.213 0.555 0.063 Uiso 0.5 1 calc PR . .
C10 C 0.294(4) 0.25 0.483(3) 0.058(8) Uani 1 2 d S . .
H10A H 0.2912 0.287 0.4193 0.07 Uiso 0.5 1 calc PR . .
H10B H 0.2912 0.213 0.4193 0.07 Uiso 0.5 1 calc PR . .
C11 C 0.456(3) 0.25 0.581(2) 0.051(7) Uani 1 2 d S . .
H11A H 0.5279 0.213 0.5619 0.061 Uiso 0.5 1 calc PR . .
H11B H 0.5279 0.287 0.5619 0.061 Uiso 0.5 1 calc PR . .
C12 C 0.402(3) 0.25 0.733(3) 0.050(7) Uani 1 2 d S . .
H12A H 0.4478 0.287 0.7858 0.06 Uiso 0.5 1 calc PR . .
H12B H 0.4478 0.213 0.7858 0.06 Uiso 0.5 1 calc PR . .
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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
O1 Ni1 O2 178.4(4) . . ?
O1 Ni1 Br3 89.5(3) . . ?
O2 Ni1 Br3 89.6(3) . . ?
O1 Ni1 Br1 90.8(3) . . ?
O2 Ni1 Br1 90.2(3) . . ?
Br3 Ni1 Br1 179.78(11) . . ?
O1 Ni1 Br1 91.0(3) . 3_567 ?
O2 Ni1 Br1 90.3(3) . 3_567 ?
Br3 Ni1 Br1 93.02(8) . 3_567 ?
Br1 Ni1 Br1 86.96(7) . 3_567 ?
O1 Ni1 Br2 89.4(3) . . ?
O2 Ni1 Br2 89.2(3) . . ?
Br3 Ni1 Br2 85.05(7) . . ?
Br1 Ni1 Br2 94.97(8) . . ?
Br1 Ni1 Br2 178.03(9) 3_567 . ?
O3 Ni2 Br3 98.8(3) . . ?
O3 Ni2 Br3 98.8(3) . 4_565 ?
Br3 Ni2 Br3 87.95(11) . 4_565 ?
O3 Ni2 Br2 97.1(3) . 4_565 ?
Br3 Ni2 Br2 164.00(14) . 4_565 ?
Br3 Ni2 Br2 87.88(5) 4_565 4_565 ?
O3 Ni2 Br2 97.1(3) . . ?
Br3 Ni2 Br2 87.88(5) . . ?
Br3 Ni2 Br2 164.00(14) 4_565 . ?
Br2 Ni2 Br2 91.91(11) 4_565 . ?
Ni1 Br1 Ni1 93.04(7) . 3_567 ?
Ni2 Br2 Ni1 92.35(8) . . ?
Ni2 Br3 Ni1 94.70(8) . . ?
C1 O1 C4 111.0(12) . . ?
C1 O1 Ni1 123.3(10) . . ?
C4 O1 Ni1 125.6(9) . . ?
C8 O2 C5 106.7(12) . . ?
C8 O2 Ni1 124.5(10) . . ?
C5 O2 Ni1 126.7(9) . . ?
C9 O3 C12 111.1(19) . . ?
C9 O3 Ni2 124.8(15) . . ?
C12 O3 Ni2 124.0(13) . . ?
O1 C1 C2 106.8(14) . . ?
C1 C2 C3 106.9(14) . . ?
C4 C3 C2 108.3(15) . . ?
O1 C4 C3 106.9(13) . . ?
O2 C5 C6 110.4(15) . . ?
C5 C6 C7 103.3(19) . . ?
C8 C7 C6 107.4(18) . . ?
O2 C8 C7 111.6(16) . . ?
O3 C9 C10 107(2) . . ?
C9 C10 C11 108.1(19) . . ?
C12 C11 C10 108(2) . . ?
C11 C12 O3 105.2(18) . . ?
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
Ni1 O1 2.108(10) . ?
Ni1 O2 2.125(10) . ?
Ni1 Br3 2.527(2) . ?
Ni1 Br1 2.529(2) . ?
Ni1 Br1 2.557(2) 3_567 ?
Ni1 Br2 2.597(2) . ?
Ni2 O3 2.009(17) . ?
Ni2 Br3 2.482(2) . ?
Ni2 Br3 2.482(2) 4_565 ?
Ni2 Br2 2.509(2) 4_565 ?
Ni2 Br2 2.509(2) . ?
Br1 Ni1 2.557(2) 3_567 ?
O1 C1 1.439(18) . ?
O1 C4 1.45(2) . ?
O2 C8 1.413(18) . ?
O2 C5 1.46(2) . ?
O3 C9 1.42(3) . ?
O3 C12 1.50(3) . ?
C1 C2 1.48(3) . ?
C2 C3 1.49(2) . ?
C3 C4 1.45(2) . ?
C5 C6 1.47(3) . ?
C6 C7 1.54(3) . ?
C7 C8 1.43(3) . ?
C9 C10 1.47(4) . ?
C10 C11 1.49(4) . ?
C11 C12 1.47(3) . ?
