#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/45/2004547.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2004547
loop_
_publ_author_name
'McLachlan, G. A.'
'Fallon, G. D.'
'Spiccia, L.'
_publ_section_title
;
 [Cr{tren(impy)₃}](ClO₄)₃, where tren(impy)₃ = N[CH₂CH₂N=
 C(H)(py)]₃
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              309
_journal_page_last               312
_journal_paper_doi               10.1107/S0108270195008870
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Cr (C24 H27 N7)] (Cl O4)3'
_chemical_formula_moiety         'C24 H27 Cr N7 , 3Cl O4'
_chemical_formula_sum            'C24 H27 Cl3 Cr N7 O12'
_chemical_formula_weight         763.9
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_type_scat_source           'IntTabIV and Cromer & Waber (1974)'
_cell_angle_alpha                90
_cell_angle_beta                 107.870(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.472(4)
_cell_length_b                   13.207(2)
_cell_length_c                   13.592(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293
_cell_measurement_theta_max      13
_cell_measurement_theta_min      3
_cell_volume                     3155.9(10)
_computing_cell_refinement
'Siemens P3/v data collection system, release 4.12'
_computing_data_collection
'Siemens P3/v data collection system, release 4.12'
_computing_data_reduction        'Shelxtl-Plus (Sheldrick, 1991)'
_computing_molecular_graphics    Shelxtl-Plus
_computing_publication_material  Shelxtl-Plus
_computing_structure_refinement  Shelxtl-Plus
_computing_structure_solution    Shelxtl-Plus
_diffrn_measurement_device       'Nicolet R3m/V'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            7131
_diffrn_reflns_theta_max         25
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.68
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            'wine red'
_exptl_crystal_density_diffrn    1.61
_exptl_crystal_density_meas      1.600(10)
_exptl_crystal_density_method    'flotation in C~2~H~2~Br~4~/CCl~4~'
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.02
_refine_diff_density_min         -0.48
_refine_ls_extinction_method
'four reflections omitted from final calculations (200, 011, 220, \=111)'
_refine_ls_goodness_of_fit_obs   1.83
_refine_ls_hydrogen_treatment    refU
_refine_ls_number_parameters     424
_refine_ls_number_reflns         3313
_refine_ls_R_factor_obs          0.056
_refine_ls_shift/esd_max         0.004
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fₒ)+0.00741Fₒ²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.074
_reflns_number_observed          3317
_reflns_number_total             5586
_reflns_observed_criterion       F>6\s(F)
_cod_data_source_file            ta1028.cif
_cod_data_source_block           ta1028a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value ' 1/[\s^2^(F~o~)+0.00741F~o~^2^]'
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^(F~o~)+0.00741F~o~^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3156.0(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2004547
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x,1/2-y,1/2+z
-x,-y,-z
-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
Cr .25855(5) .52190(7) .17161(7) .0323(3)
N(1) .2802(3) .4799(4) .3235(3) .037(2)
N(2) .1632(3) .5756(4) .2007(4) .040(2)
N(3) .1977(3) .7389(4) .0895(4) .048(2)
N(4) .3273(3) .6458(4) .2180(3) .037(2)
N(5) .3601(3) .4668(4) .1599(3) .037(2)
N(6) .2239(3) .5479(3) .0164(3) .035(2)
N(7) .1975(3) .3915(4) .1170(3) .036(2)
C(1) .3417(4) .4355(5) .3856(5) .048(2)
C(2) .3468(4) .4096(6) .4867(5) .062(3)
C(3) .2881(5) .4313(6) .5241(5) .066(3)
C(4) .2242(4) .4790(5) .4613(5) .049(2)
C(5) .2221(3) .5029(5) .3620(5) .040(2)
C(6) .1593(3) .5554(5) .2900(5) .043(2)
C(7) .1008(3) .6326(5) .1275(5) .054(3)
C(8) .1272(4) .7396(5) .1163(6) .061(3)
C(9) .2588(4) .8002(5) .1528(5) .053(3)
C(10) .3035(4) .7449(5) .2469(5) .051(3)
C(11) .3949(3) .6332(5) .2148(5) .044(2)
C(12) .4156(3) .5377(5) .1808(4) .040(2)
C(13) .4855(3) .5190(5) .1676(5) .050(2)
C(14) .4983(4) .4249(6) .1331(6) .059(3)
C(15) .4432(4) .3535(6) .1126(5) .058(3)
C(16) .3746(4) .3761(5) .1281(5) .046(2)
C(17) .1916(4) .7251(5) -.0182(5) .057(3)
C(18) .2414(4) .6406(5) -.0341(5) .049(2)
C(19) .1836(3) .4793(5) -.0390(4) .040(2)
C(20) .1652(3) .3906(5) .0122(4) .040(2)
C(21) .1201(3) .3125(5) -.0387(5) .049(3)
C(22) .1059(4) .2331(6) .0182(6) .060(3)
C(23) .1387(4) .2317(5) .1230(6) .058(3)
C(24) .1846(4) .3128(5) .1697(5) .050(3)
Cl(1) .30310(10) .39440(10) .82410(10) .0560(10)
O(1) .2711(3) .3266(4) .8808(4) .082(3)
O(2) .2422(3) .4489(5) .7537(4) .091(3)
O(3) .3424(3) .3397(5) .7676(4) .085(3)
O(4) .3524(3) .4628(5) .8940(4) .099(3)
Cl(2) .43610(10) .67920(10) .52260(10) .0560(10)
O(5) .4709(3) .6435(5) .4497(5) .096(3)
O(6) .4379(4) .7863(4) .5266(6) .111(4)
O(7) .3567(3) .6535(5) .4812(5) .101(3)
O(8) .4642(5) .6342(8) .6156(5) .170(5)
Cl(3) -.00310(10) .3765(2) .2230(2) .0910(10)
O(9) -.0596(6) .4222(8) .2486(7) .175(6)
O(10) -.0210(5) .2687(7) .2143(7) .159(5)
O(11) .0004(4) .4136(7) .1263(5) .133(4)
O(12) .0673(3) .3829(6) .2970(5) .121(3)
H(1A) .3830 .4196 .3592 .080
H(2A) .3917 .3772 .5303 .080
H(3A) .2914 .4132 .5938 .080
H(4A) .1820 .4944 .4861 .080
H(6A) .1154 .5742 .3095 .080
H(7A) .0569 .6328 .1512 .080
H(7B) .0874 .5998 .0613 .080
H(8A) .0887 .7745 .0636 .080
H(8B) .1346 .7747 .1805 .080
H(9A) .2381 .8608 .1725 .080
H(9B) .2916 .8193 .1130 .080
H(10A) .3478 .7832 .2832 .080
H(10B) .2731 .7354 .2923 .080
H(11A) .4312 .6873 .2343 .080
H(13A) .5243 .5701 .1831 .080
H(14A) .5460 .4103 .1216 .080
H(15A) .4521 .2878 .0884 .080
H(16A) .3364 .3244 .1157 .080
H(17A) .2057 .7870 -0.0445 .080
H(17B) .1397 .7105 -0.0565 .080
H(18A) .2322 .6280 -0.1065 .080
H(18B) .2940 .6585 -0.0040 .080
H(19A) .1646 .4863 -0.1128 .080
H(21A) .0984 .3140 -0.1125 .080
H(22A) .0730 .1788 -0.0153 .080
H(23A) .1308 .1758 .1637 .080
H(24A) .2080 .3122 .2433 .080
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N(1) Cr N(2) 79.3(2) yes
N(2) Cr N(4) 98.8(2) yes
N(2) Cr N(5) 173.6(2) yes
N(1) Cr N(6) 171.3(2) yes
N(4) Cr N(6) 98.7(2) yes
N(1) Cr N(7) 93.0(2) yes
N(4) Cr N(7) 173.8(2) yes
N(6) Cr N(7) 78.8(2) yes
Cr N(1) C(5) 113.0(3) yes
Cr N(2) C(6) 114.7(4) yes
C(6) N(2) C(7) 119.4(6) yes
C(8) N(3) C(17) 117.2(5) yes
Cr N(4) C(10) 125.7(4) yes
C(10) N(4) C(11) 120.2(5) yes
N(1) C(5) C(4) 122.5(5) yes
N(2) C(7) C(8) 109.4(5) yes
N(3) C(9) C(10) 111.4(5) yes
N(4) C(11) C(12) 119.2(6) yes
N(1) Cr N(4) 89.7(2) yes
N(1) Cr N(5) 94.6(2) yes
N(4) Cr N(5) 79.2(2) yes
N(2) Cr N(6) 97.2(2) yes
N(5) Cr N(6) 89.1(2) yes
N(2) Cr N(7) 87.2(2) yes
N(5) Cr N(7) 95.0(2) yes
Cr N(1) C(1) 128.6(5) yes
C(1) N(1) C(5) 118.4(5) yes
Cr N(2) C(7) 125.9(4) yes
C(8) N(3) C(9) 116.3(6) yes
C(9) N(3) C(17) 118.6(6) yes
Cr N(4) C(11) 114.0(4) yes
N(1) C(1) C(2) 121.5(7) yes
N(1) C(5) C(6) 114.2(5) yes
N(2) C(6) C(5) 118.7(6) yes
N(3) C(8) C(7) 111.0(6) yes
N(4) C(10) C(9) 109.9(5) yes
Cr N(5) C(16) 128.5(4) no
Cr N(6) C(18) 125.0(3) no
C(18) N(6) C(19) 119.2(5) no
Cr N(7) C(24) 128.9(4) no
C(2) C(3) C(4) 119.5(7) no
C(4) C(5) C(6) 123.3(6) no
N(5) C(12) C(13) 121.9(6) no
C(12) C(13) C(14) 118.2(6) no
Cr N(5) C(12) 112.9(4) no
C(12) N(5) C(16) 118.5(5) no
Cr N(6) C(19) 115.8(4) no
Cr N(7) C(20) 113.4(4) no
C(20) N(7) C(24) 117.6(5) no
C(1) C(2) C(3) 119.8(6) no
C(3) C(4) C(5) 118.2(7) no
N(5) C(12) C(11) 114.6(6) no
C(11) C(12) C(13) 123.5(6) no
C(13) C(14) C(15) 120.2(7) no
C(14) C(15) C(16) 119.1(7) no
N(3) C(17) C(18) 112.2(5) no
N(6) C(19) C(20) 118.3(5) no
N(7) C(20) C(21) 122.4(6) no
C(20) C(21) C(22) 118.7(6) no
C(22) C(23) C(24) 118.6(7) no
O(1) Cl(1) O(2) 108.0(4) no
O(2) Cl(1) O(3) 109.0(3) no
O(2) Cl(1) O(4) 109.8(4) no
O(5) Cl(2) O(6) 110.4(5) no
O(6) Cl(2) O(7) 105.0(4) no
O(6) Cl(2) O(8) 114.0(5) no
O(9) Cl(3) O(10) 106.6(6) no
O(10) Cl(3) O(11) 109.5(5) no
O(10) Cl(3) O(12) 105.0(5) no
N(5) C(16) C(15) 122.1(6) no
N(6) C(18) C(17) 108.4(6) no
N(7) C(20) C(19) 113.6(5) no
C(19) C(20) C(21) 123.9(5) no
C(21) C(22) C(23) 119.8(6) no
N(7) C(24) C(23) 122.8(6) no
O(1) Cl(1) O(3) 110.0(4) no
O(3) Cl(1) O(4) 111.0(4) no
O(5) Cl(2) O(7) 105.9(4) no
O(5) Cl(2) O(8) 112.5(5) no
O(7) Cl(2) O(8) 108.4(5) no
O(9) Cl(3) O(11) 110.1(6) no
O(9) Cl(3) O(12) 114.7(5) no
O(11) Cl(3) O(12) 110.6(4) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cr N(1) 2.055(5) yes
Cr N(4) 2.049(5) yes
Cr N(6) 2.037(5) yes
N(1) C(1) 1.325(7) yes
N(2) C(6) 1.267(9) yes
N(3) C(8) 1.456(10) yes
N(3) C(17) 1.444(9) yes
N(4) C(11) 1.273(9) yes
Cr N(2) 2.046(5) yes
Cr N(5) 2.063(5) yes
Cr N(7) 2.067(5) yes
N(1) C(5) 1.364(9) yes
N(2) C(7) 1.477(7) yes
N(3) C(9) 1.440(8) yes
N(4) C(10) 1.472(8) yes
N(5) C(16) 1.329(8) no
N(6) C(19) 1.265(7) no
N(7) C(24) 1.325(9) no
C(2) C(3) 1.363(13) no
C(4) C(5) 1.376(9) no
C(7) C(8) 1.518(10) no
C(11) C(12) 1.434(9) no
C(13) C(14) 1.374(11) no
C(15) C(16) 1.378(11) no
C(19) C(20) 1.455(9) no
C(21) C(22) 1.376(11) no
C(23) C(24) 1.392(9) no
Cl(1) O(2) 1.427(6) no
Cl(1) O(4) 1.421(6) no
Cl(2) O(6) 1.416(6) no
Cl(2) O(8) 1.349(8) no
Cl(3) O(10) 1.458(10) no
Cl(3) O(12) 1.380(6) no
N(5) C(12) 1.353(8) no
N(6) C(18) 1.486(8) no
N(7) C(20) 1.364(7) no
C(1) C(2) 1.391(10) no
C(3) C(4) 1.379(10) no
C(5) C(6) 1.445(8) no
C(9) C(10) 1.484(8) no
C(12) C(13) 1.379(9) no
C(14) C(15) 1.354(10) no
C(17) C(18) 1.503(10) no
C(20) C(21) 1.372(8) no
C(22) C(23) 1.366(10) no
Cl(1) O(1) 1.422(6) no
Cl(1) O(3) 1.408(7) no
Cl(2) O(5) 1.417(7) no
Cl(2) O(7) 1.441(6) no
Cl(3) O(9) 1.342(11) no
Cl(3) O(11) 1.423(8) no
