#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/84/4318474.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_4318474
loop_
_publ_author_name
'Robertus J. M. Klein Gebbink'
'Robert T. Jonas'
'Christian R. Goldsmith'
'T. Daniel P. Stack'
_publ_section_title
;
 A Periodic Walk: A Series of First-Row Transition Metal Complexes with
 the Pentadentate Ligand PY5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4633
_journal_page_last               4641
_journal_paper_doi               10.1021/ic025617r
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C29 H27 Cl3 N5 O3 Zn1.5'
_chemical_formula_weight         697.99
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 93.648(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7075(3)
_cell_length_b                   14.5730(2)
_cell_length_c                   18.7159(5)
_cell_measurement_reflns_used    4695
_cell_measurement_temperature    175
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      1.39
_cell_volume                     2914.52(12)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_publication_material  'teXsan for Windows (MSC, 1997)'
_computing_structure_refinement  'teXsan for Windows (MSC, 1997)'
_computing_structure_solution
;

SHELXS86 (Sheldrick, 1985)

;
_diffrn_ambient_temperature      175
_diffrn_measurement_device       unknown
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.07162
_diffrn_reflns_av_sigmaI/netI    0.174
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13817
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         1.39
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.560
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1424.00
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.48
_refine_diff_density_min         -1.81
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.678
_refine_ls_goodness_of_fit_ref   1.680
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5108
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1642
_refine_ls_shift/su_max          0.5300
_refine_ls_shift/su_mean         0.0138
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00022|Fo|²]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.1910
_reflns_number_gt                5108
_reflns_number_total             5344
_reflns_threshold_expression     I>0.00σ(I)
_cod_data_source_file            ic025617r_5.cif
_cod_data_source_block           '_rtj64'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2914.5(1)
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_original_formula_sum        'C29 H27 Cl3 N5 O3 Zn1.50 '
_cod_database_code               4318474
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
_atom_site_occupancy
_atom_site_refinement_flags
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
Zn(1) 0.17523(8) -0.40296(6) 0.30971(5) 0.0207(2) 1.000 . Uani d ?
Zn(2) 0.5255(2) 0.4875(2) 0.0266(1) 0.0578(8) 0.500 S Uani d ?
Cl(1) 0.3414(2) -0.3110(1) 0.2824(1) 0.0313(6) 1.000 . Uani d ?
Cl(2) 0.6737(3) 0.4093(3) 0.0936(2) 0.0294(9) 0.500 S Uiso d ?
Cl(3) 0.4777(6) 0.6101(4) 0.0876(3) 0.085(2) 0.500 S Uiso d ?
Cl(4) 0.603(1) 0.5408(9) -0.0784(7) 0.224(5) 0.500 S Uiso d ?
Cl(5) 0.3310(7) 0.4101(6) 0.0254(4) 0.124(3) 0.500 S Uiso d ?
O(1) 0.1754(5) -0.6593(3) 0.4560(3) 0.027(2) 1.000 . Uani d ?
O(2) -0.2421(4) -0.3930(4) 0.2288(3) 0.029(2) 1.000 . Uani d ?
O(3) 0.4141(6) 0.2234(5) 0.0857(4) 0.094(3) 1.000 . Uani d ?
N(1) 0.0227(5) -0.4923(4) 0.3351(3) 0.015(2) 1.000 . Uani d ?
N(2) 0.2850(5) -0.5346(4) 0.3069(3) 0.019(2) 1.000 . Uani d ?
N(3) 0.2261(5) -0.4153(4) 0.4249(3) 0.021(2) 1.000 . Uani d ?
N(4) 0.0403(5) -0.2955(4) 0.3196(3) 0.017(2) 1.000 . Uani d ?
N(5) 0.0850(5) -0.4041(4) 0.1969(3) 0.021(2) 1.000 . Uani d ?
C(1) 0.0510(6) -0.5724(5) 0.3685(3) 0.016(2) 1.000 . Uani d ?
C(2) -0.0244(7) -0.6490(5) 0.3592(4) 0.024(2) 1.000 . Uani d ?
C(3) -0.1307(7) -0.6434(5) 0.3154(4) 0.030(3) 1.000 . Uani d ?
C(4) -0.1629(7) -0.5617(5) 0.2817(4) 0.028(2) 1.000 . Uani d ?
C(5) -0.0852(6) -0.4862(5) 0.2935(4) 0.018(2) 1.000 . Uani d ?
C(6) 0.1788(6) -0.5811(5) 0.4113(4) 0.019(2) 1.000 . Uani d ?
C(7) 0.0902(8) -0.6536(6) 0.5125(4) 0.039(3) 1.000 . Uani d ?
C(8) 0.2769(6) -0.6002(5) 0.3575(4) 0.020(2) 1.000 . Uani d ?
C(9) 0.3525(7) -0.6777(5) 0.3611(4) 0.026(2) 1.000 . Uani d ?
C(10) 0.4419(6) -0.6873(5) 0.3117(4) 0.026(2) 1.000 . Uani d ?
C(11) 0.4544(7) -0.6205(5) 0.2602(4) 0.029(2) 1.000 . Uani d ?
C(12) 0.3749(7) -0.5450(5) 0.2594(4) 0.029(2) 1.000 . Uani d ?
C(13) 0.2321(6) -0.4981(5) 0.4548(4) 0.020(2) 1.000 . Uani d ?
C(14) 0.3001(7) -0.5148(5) 0.5196(4) 0.032(2) 1.000 . Uani d ?
C(15) 0.3567(8) -0.4417(6) 0.5562(4) 0.036(3) 1.000 . Uani d ?
C(16) 0.3463(8) -0.3555(6) 0.5263(4) 0.038(3) 1.000 . Uani d ?
C(17) 0.2818(7) -0.3444(5) 0.4604(4) 0.031(2) 1.000 . Uani d ?
C(18) -0.1145(6) -0.3947(5) 0.2536(4) 0.020(2) 1.000 . Uani d ?
C(19) -0.337(1) -0.4028(7) 0.2817(6) 0.089(4) 1.000 . Uani d ?
C(20) -0.0398(7) -0.3967(5) 0.1855(4) 0.021(2) 1.000 . Uani d ?
C(21) -0.1008(7) -0.3921(5) 0.1184(4) 0.024(2) 1.000 . Uani d ?
C(22) -0.0276(8) -0.3938(6) 0.0592(4) 0.035(3) 1.000 . Uani d ?
C(23) 0.1012(8) -0.3991(6) 0.0703(4) 0.035(3) 1.000 . Uani d ?
C(24) 0.1542(7) -0.4044(5) 0.1389(4) 0.028(2) 1.000 . Uani d ?
C(25) -0.0797(7) -0.3062(5) 0.2955(4) 0.019(2) 1.000 . Uani d ?
C(26) -0.1654(7) -0.2362(5) 0.3029(4) 0.026(2) 1.000 . Uani d ?
C(27) -0.1315(7) -0.1562(5) 0.3376(4) 0.028(2) 1.000 . Uani d ?
C(28) -0.0084(7) -0.1452(5) 0.3605(4) 0.025(2) 1.000 . Uani d ?
C(29) 0.0735(7) -0.2153(5) 0.3498(4) 0.023(2) 1.000 . Uani d ?
H(1) -0.0017 -0.7049 0.3826 0.029 1.000 . Uiso c ?
H(2) -0.1844 -0.6953 0.3086 0.037 1.000 . Uiso c ?
H(3) -0.2360 -0.5577 0.2500 0.036 1.000 . Uiso c ?
H(4) 0.1127 -0.6032 0.5423 0.046 1.000 . Uiso c ?
H(5) 0.0079 -0.6466 0.4921 0.046 1.000 . Uiso c ?
H(6) 0.0961 -0.7089 0.5399 0.046 1.000 . Uiso c ?
H(7) 0.3428 -0.7223 0.3979 0.032 1.000 . Uiso c ?
H(8) 0.4955 -0.7407 0.3137 0.035 1.000 . Uiso c ?
H(9) 0.5157 -0.6262 0.2264 0.037 1.000 . Uiso c ?
H(10) 0.3837 -0.5001 0.2237 0.033 1.000 . Uiso c ?
H(11) 0.3076 -0.5748 0.5383 0.040 1.000 . Uiso c ?
H(12) 0.4013 -0.4511 0.6011 0.047 1.000 . Uiso c ?
H(13) 0.3847 -0.3038 0.5501 0.048 1.000 . Uiso c ?
H(14) 0.2770 -0.2853 0.4400 0.037 1.000 . Uiso c ?
H(15) -0.3278 -0.3545 0.3172 0.128 1.000 . Uiso c ?
H(16) -0.4192 -0.3991 0.2596 0.128 1.000 . Uiso c ?
H(17) -0.3274 -0.4600 0.3062 0.128 1.000 . Uiso c ?
H(18) -0.1889 -0.3871 0.1122 0.032 1.000 . Uiso c ?
H(19) -0.0656 -0.3910 0.0125 0.041 1.000 . Uiso c ?
H(20) 0.1532 -0.3999 0.0307 0.043 1.000 . Uiso c ?
H(21) 0.2425 -0.4082 0.1459 0.034 1.000 . Uiso c ?
H(22) -0.2500 -0.2451 0.2846 0.030 1.000 . Uiso c ?
H(23) -0.1908 -0.1100 0.3447 0.037 1.000 . Uiso c ?
H(24) 0.0193 -0.0896 0.3835 0.031 1.000 . Uiso c ?
H(25) 0.1592 -0.2064 0.3653 0.029 1.000 . Uiso c ?
H(26) 0.4102 0.2813 0.0616 0.119 1.000 . Uiso c ?
H(28) 0.4921 0.1943 0.0744 0.119 1.000 . Uiso c ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 116 0.002 0.002
;International Tables for Crystallography

(1992, Vol. C, Table 6.1.1.2)

;
H 0 108 0.000 0.000
;International Tables for Crystallography

(1992, Vol. C, Table 6.1.1.2)

;
N 0 20 0.004 0.003
;International Tables for Crystallography

(1992, Vol. C, Table 6.1.1.2)

;
O 0 12 0.008 0.006
;International Tables for Crystallography

(1992, Vol. C, Table 6.1.1.2)

;
Cl 0 12 0.132 0.159
;International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)

;
Zn 0 6 0.222 1.431
;International Tables for Crystallography

(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)

;
