#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:53:40 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178922 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/51/4115179.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_4115179
loop_
_publ_author_name
'Louise A. Berben'
'Jeffrey R. Long'
_publ_contact_author
;
        Jeffrey R. Long
        Department of Chemistry
        University of California, Berkeley
        United States of America
;
_publ_contact_author_email       jlong@cchem.berkeley.edu
_publ_contact_author_fax         '510 643-3832'
_publ_contact_author_phone       '510 642-0860'
_publ_section_title
;
 Synthesis and Alkali Metal Ion-Binding Properties of a Chromium(III)
 Triacetylide Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11588
_journal_page_last               11589
_journal_paper_doi               10.1021/ja027309y
_journal_volume                  124
_journal_year                    2002
_chemical_compound_source        synthetic
_chemical_formula_structural
;
 [(C9H21N3)Cr(C2H)3]CsBr-2(H2O)
;
_chemical_formula_sum            'C45 H76 Br Cr3 Cs N9 O2'
_chemical_formula_weight         1143.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      176
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   16.1420(9)
_cell_length_b                   16.1420(9)
_cell_length_c                   11.8364(9)
_cell_measurement_temperature    120(2)
_cell_volume                     2670.9(3)
_computing_cell_refinement
;
  SMART (Siemens, 1995), SAINT (Siemens, 1995)
;
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction
;
  SAINT (Siemens, 1995), XPREP (Siemens, 1995)
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       'omega scans with profile analysis'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0354
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11997
_diffrn_reflns_theta_max         25.43
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    2.061
_exptl_absorpt_correction_T_max  2.061
_exptl_absorpt_correction_T_min  1
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       rod
_exptl_crystal_F_000             1174
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.081
_refine_diff_density_min         -1.124
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_all   1.078
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_obs          0.0481
_refine_ls_shift/esd_max         -2.932
_refine_ls_shift/esd_mean        0.085
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1311P)²+7.1103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1356
_refine_ls_wR_factor_obs         0.1238
_reflns_number_observed          1329
_reflns_number_total             1666
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja027309y_s2_3.cif
_cod_data_source_block           lab28a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
calc w=1/[\s^2^(Fo^2^)+(0.1311P)^2^+7.1103P] 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^)+(0.1311P)^2^+7.1103P] 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               4115179
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cs1 Cs 0.3333 0.6667 0.7500 0.0345(3) Uani 1 d S
Cr1 Cr 0.61270(10) 0.92828(8) 0.7500 0.0403(4) Uani 1 d S
C1 C 0.5326(4) 0.8400(3) 0.6207(4) 0.0340(12) Uani 1 d .
C2 C 0.4870(4) 0.7933(4) 0.5408(5) 0.0357(12) Uani 1 d .
H2 H 0.4518(42) 0.7572(42) 0.4791(48) 0.043 Uiso 1 calc .
C3 C 0.7017(7) 0.8741(8) 0.7500 0.056(2) Uani 1 d S
C4 C 0.7553(11) 0.8461(13) 0.7500 0.097(5) Uani 1 d S
H4 H 0.7983(97) 0.8237(96) 0.7500(11357848) 0.116 Uiso 1 calc S
N1 N 0.6977(4) 1.0425(4) 0.6305(4) 0.070(2) Uani 1 d .
N2 N 0.5261(7) 0.9993(5) 0.7500 0.063(2) Uani 1 d S
C5 C 0.6331(8) 1.0790(9) 0.5919(13) 0.149(6) Uani 1 d .
H5A H 0.6719(8) 1.1482(9) 0.5878(13) 0.178 Uiso 1 calc R
H5B H 0.6139(8) 1.0564(9) 0.5152(13) 0.178 Uiso 1 calc R
C6 C 0.5544(8) 1.0594(7) 0.6481(7) 0.100(3) Uani 1 d .
H6A H 0.5015(8) 1.0293(7) 0.5951(7) 0.119 Uiso 1 calc R
H6B H 0.5600(8) 1.1201(7) 0.6694(7) 0.119 Uiso 1 calc R
C7 C 0.7806(7) 1.1160(7) 0.6901(7) 0.146(6) Uani 1 d .
H7A H 0.8358(7) 1.1120(7) 0.6654(7) 0.175 Uiso 1 calc R
H7B H 0.7903(7) 1.1775(7) 0.6654(7) 0.175 Uiso 1 calc R
C8 C 0.7320(7) 1.0097(6) 0.5331(6) 0.092(3) Uani 1 d .
H8A H 0.7697(42) 1.0628(12) 0.4840(31) 0.138 Uiso 1 calc R
H8B H 0.6781(7) 0.9613(36) 0.4922(35) 0.138 Uiso 1 calc R
H8C H 0.7705(42) 0.9838(46) 0.5602(7) 0.138 Uiso 1 calc R
C9 C 0.4201(9) 0.9329(8) 0.7500 0.085(4) Uani 1 d S
Br1 Br 0.3333 0.6667 0.2500 0.0308(3) Uani 1 d S
O1 O 1.0000 1.0000 0.7500 0.254(18) Uiso 1 d S
O2 O 1.0000 1.0000 0.5000 0.340(27) Uiso 1 d S
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
C2 Cs1 C2 94.4(2) 2_665 11_667
C2 Cs1 C2 72.1(2) 2_665 .
C2 Cs1 C2 140.27(8) 11_667 .
C2 Cs1 C2 140.27(8) 2_665 10_557
C2 Cs1 C2 72.1(2) 11_667 10_557
C2 Cs1 C2 94.4(2) . 10_557
C2 Cs1 C2 72.1(2) 2_665 3_565
C2 Cs1 C2 140.27(8) 11_667 3_565
C2 Cs1 C2 72.1(2) . 3_565
C2 Cs1 C2 140.27(8) 10_557 3_565
C2 Cs1 C2 140.27(8) 2_665 12_567
C2 Cs1 C2 72.1(2) 11_667 12_567
C2 Cs1 C2 140.27(8) . 12_567
C2 Cs1 C2 72.1(2) 10_557 12_567
C2 Cs1 C2 94.4(2) 3_565 12_567
C2 Cs1 C1 20.48(13) 2_665 2_665
C2 Cs1 C1 74.04(13) 11_667 2_665
C2 Cs1 C1 89.77(13) . 2_665
C2 Cs1 C1 131.14(12) 10_557 2_665
C2 Cs1 C1 87.02(13) 3_565 2_665
C2 Cs1 C1 127.58(12) 12_567 2_665
C2 Cs1 C1 74.04(13) 2_665 11_667
C2 Cs1 C1 20.48(13) 11_667 11_667
C2 Cs1 C1 131.14(12) . 11_667
C2 Cs1 C1 89.77(13) 10_557 11_667
C2 Cs1 C1 127.58(12) 3_565 11_667
C2 Cs1 C1 87.02(13) 12_567 11_667
C1 Cs1 C1 53.6(2) 2_665 11_667
C2 Cs1 C1 127.58(12) 2_665 10_557
C2 Cs1 C1 87.02(13) 11_667 10_557
C2 Cs1 C1 74.04(13) . 10_557
C2 Cs1 C1 20.48(13) 10_557 10_557
C2 Cs1 C1 131.13(12) 3_565 10_557
C2 Cs1 C1 89.77(13) 12_567 10_557
C1 Cs1 C1 127.00(5) 2_665 10_557
C1 Cs1 C1 101.23(11) 11_667 10_557
C2 Cs1 C1 87.02(13) 2_665 .
C2 Cs1 C1 127.58(12) 11_667 .
C2 Cs1 C1 20.48(13) . .
C2 Cs1 C1 74.04(13) 10_557 .
C2 Cs1 C1 89.77(13) 3_565 .
C2 Cs1 C1 131.13(12) 12_567 .
C1 Cs1 C1 101.23(11) 2_665 .
C1 Cs1 C1 127.00(5) 11_667 .
C1 Cs1 C1 53.6(2) 10_557 .
C2 Cs1 C1 89.77(13) 2_665 3_565
C2 Cs1 C1 131.14(12) 11_667 3_565
C2 Cs1 C1 87.02(13) . 3_565
C2 Cs1 C1 127.58(12) 10_557 3_565
C2 Cs1 C1 20.48(13) 3_565 3_565
C2 Cs1 C1 74.04(13) 12_567 3_565
C1 Cs1 C1 101.23(11) 2_665 3_565
C1 Cs1 C1 126.99(5) 11_667 3_565
C1 Cs1 C1 126.99(5) 10_557 3_565
C1 Cs1 C1 101.23(11) . 3_565
C2 Cs1 C1 131.13(13) 2_665 12_567
C2 Cs1 C1 89.77(13) 11_667 12_567
C2 Cs1 C1 127.58(12) . 12_567
C2 Cs1 C1 87.02(13) 10_557 12_567
C2 Cs1 C1 74.04(13) 3_565 12_567
C2 Cs1 C1 20.48(13) 12_567 12_567
C1 Cs1 C1 126.99(5) 2_665 12_567
C1 Cs1 C1 101.23(11) 11_667 12_567
C1 Cs1 C1 101.23(11) 10_557 12_567
C1 Cs1 C1 126.99(4) . 12_567
C1 Cs1 C1 53.6(2) 3_565 12_567
C3 Cr1 C1 92.1(2) . .
C3 Cr1 C1 92.1(2) . 10_557
C1 Cr1 C1 96.6(3) . 10_557
C3 Cr1 N1 94.8(3) . 10_557
C1 Cr1 N1 169.7(2) . 10_557
C1 Cr1 N1 90.8(2) 10_557 10_557
C3 Cr1 N1 94.8(3) . .
C1 Cr1 N1 90.8(2) . .
C1 Cr1 N1 169.7(2) 10_557 .
N1 Cr1 N1 80.9(3) 10_557 .
C3 Cr1 N2 175.3(4) . .
C1 Cr1 N2 91.0(2) . .
C1 Cr1 N2 91.0(2) 10_557 .
N1 Cr1 N2 81.7(3) 10_557 .
N1 Cr1 N2 81.7(3) . .
C3 Cr1 Cs1 101.2(3) . .
C1 Cr1 Cs1 48.80(14) . .
C1 Cr1 Cs1 48.80(14) 10_557 .
N1 Cr1 Cs1 136.52(15) 10_557 .
N1 Cr1 Cs1 136.5(2) . .
N2 Cr1 Cs1 83.5(2) . .
C2 C1 Cr1 175.9(4) . .
C2 C1 Cs1 78.9(3) . .
Cr1 C1 Cs1 104.2(2) . .
C1 C2 Cs1 80.6(4) . .
C4 C3 Cr1 177.7(12) . .
C7 N1 C8 108.2(7) . .
C7 N1 C5 111.3(9) . .
C8 N1 C5 111.1(8) . .
C7 N1 Cr1 108.0(5) . .
C8 N1 Cr1 113.0(4) . .
C5 N1 Cr1 105.2(5) . .
C6 N2 C6 110.3(9) 10_557 .
C6 N2 C9 109.8(7) 10_557 .
C6 N2 C9 109.8(7) . .
C6 N2 Cr1 105.9(6) 10_557 .
C6 N2 Cr1 105.9(6) . .
C9 N2 Cr1 114.9(5) . .
C6 C5 N1 121.7(8) . .
C5 C6 N2 120.9(9) . .
C7 C7 N1 119.1(4) 10_557 .
N2 C9 Cs1 117.0(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cs1 C2 3.375(5) 2_665
Cs1 C2 3.375(5) 11_667
Cs1 C2 3.375(5) .
Cs1 C2 3.375(5) 10_557
Cs1 C2 3.375(5) 3_565
Cs1 C2 3.375(5) 12_567
Cs1 C1 3.394(5) 2_665
Cs1 C1 3.394(5) 11_667
Cs1 C1 3.394(5) 10_557
Cs1 C1 3.394(5) .
Cs1 C1 3.394(5) 3_565
Cs1 C1 3.394(5) 12_567
Cr1 C3 2.022(10) .
Cr1 C1 2.050(5) .
Cr1 C1 2.050(5) 10_557
Cr1 N1 2.180(5) 10_557
Cr1 N1 2.180(5) .
Cr1 N2 2.208(8) .
C1 C2 1.203(8) .
C3 C4 1.16(2) .
N1 C7 1.452(9) .
N1 C8 1.486(10) .
N1 C5 1.503(12) .
N2 C6 1.471(9) 10_557
N2 C6 1.471(9) .
N2 C9 1.50(2) .
C5 C6 1.325(14) .
C7 C7 1.42(2) 10_557
