#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:32:07 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180043 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/37/7033764.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_7033764
loop_
_publ_author_name
'Hwang, Eun Yeong'
'Park, Geun Ho'
'Lee, Chun Sun'
'Kang, Yi Young'
'Lee, Junseong'
'Lee, Bun Yeoul'
_publ_section_title
;
 Preparation of octahydro- and tetrahydro-[1,10]phenanthroline zirconium
 and hafnium complexes for olefin polymerization.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3845
_journal_page_last               3855
_journal_paper_doi               10.1039/c4dt03683b
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C16 H28 Cl2 N4 Zr'
_chemical_formula_weight         438.54
_chemical_name_systematic
; 
 ? 
;
_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_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-12 deposited with the CCDC.
2015-01-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.536(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4242(3)
_cell_length_b                   27.2768(9)
_cell_length_c                   9.1772(3)
_cell_measurement_reflns_used    7844
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.49
_cell_measurement_theta_min      2.58
_cell_volume                     1974.78(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13841
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.8854
_exptl_absorpt_correction_T_min  0.7885
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.663
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.3010P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                3697
_reflns_number_total             4076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03683b2.cif
_cod_data_source_block           lby56-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7033764--7033768.cif.
;
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               7033764
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zr1 Zr 0.30293(3) 0.583920(10) 0.60561(3) 0.02285(14) Uani 1 1 d .
Cl1 Cl 0.56341(10) 0.56051(3) 0.82395(10) 0.0439(2) Uani 1 1 d .
Cl2 Cl 0.23059(9) 0.49929(3) 0.48650(9) 0.0332(2) Uani 1 1 d .
H3N H 0.543(5) 0.5685(15) 0.485(5) 0.035(11) Uiso 1 1 d .
H4N H 0.063(5) 0.5439(15) 0.687(5) 0.040(11) Uiso 1 1 d .
N1 N 0.3167(3) 0.65761(9) 0.6712(3) 0.0264(5) Uani 1 1 d .
N2 N 0.0981(3) 0.61632(9) 0.4316(3) 0.0252(5) Uani 1 1 d .
N3 N 0.4869(4) 0.58984(11) 0.4644(4) 0.0337(6) Uani 1 1 d .
N4 N 0.1295(4) 0.55897(11) 0.7454(3) 0.0327(6) Uani 1 1 d .
C1 C 0.4285(5) 0.68082(13) 0.8153(4) 0.0451(9) Uani 1 1 d .
H1A H 0.5303 0.6601 0.8617 0.054 Uiso 1 1 calc R
H1B H 0.3685 0.6827 0.8905 0.054 Uiso 1 1 calc R
C2 C 0.4832(5) 0.73145(14) 0.7889(5) 0.0505(10) Uani 1 1 d .
H2A H 0.5609 0.7449 0.8885 0.061 Uiso 1 1 calc R
H2B H 0.5454 0.7298 0.7153 0.061 Uiso 1 1 calc R
C3 C 0.3325(4) 0.76463(12) 0.7243(4) 0.0376(7) Uani 1 1 d .
H3A H 0.2859 0.7725 0.8067 0.045 Uiso 1 1 calc R
H3B H 0.3678 0.7957 0.6888 0.045 Uiso 1 1 calc R
C4 C 0.1986(4) 0.74035(11) 0.5905(4) 0.0289(6) Uani 1 1 d .
C5 C 0.1984(3) 0.68983(10) 0.5702(3) 0.0224(6) Uani 1 1 d .
C6 C 0.0734(4) 0.76754(12) 0.4796(4) 0.0386(8) Uani 1 1 d .
H6 H 0.0702 0.8021 0.4919 0.046 Uiso 1 1 calc R
C7 C -0.0454(4) 0.74582(12) 0.3533(4) 0.0381(8) Uani 1 1 d .
H7 H -0.1286 0.7656 0.2802 0.046 Uiso 1 1 calc R
C8 C -0.0464(3) 0.69538(12) 0.3303(3) 0.0288(6) Uani 1 1 d .
C9 C 0.0778(3) 0.66733(11) 0.4402(3) 0.0235(6) Uani 1 1 d .
C10 C -0.1687(4) 0.67141(13) 0.1888(4) 0.0359(7) Uani 1 1 d .
H10A H -0.1919 0.6935 0.0980 0.043 Uiso 1 1 calc R
H10B H -0.2771 0.6650 0.2049 0.043 Uiso 1 1 calc R
C11 C -0.0945(5) 0.62348(14) 0.1578(4) 0.0477(9) Uani 1 1 d .
H11A H -0.1818 0.6054 0.0739 0.057 Uiso 1 1 calc R
H11B H 0.0015 0.6305 0.1224 0.057 Uiso 1 1 calc R
C12 C -0.0342(5) 0.59249(13) 0.3018(4) 0.0410(8) Uani 1 1 d .
H12A H -0.1317 0.5847 0.3342 0.049 Uiso 1 1 calc R
H12B H 0.0106 0.5612 0.2774 0.049 Uiso 1 1 calc R
C13 C 0.4099(6) 0.58441(15) 0.2936(5) 0.0494(10) Uani 1 1 d .
H13A H 0.3274 0.6108 0.2512 0.074 Uiso 1 1 calc R
H13B H 0.3525 0.5526 0.2686 0.074 Uiso 1 1 calc R
H13C H 0.4986 0.5863 0.2476 0.074 Uiso 1 1 calc R
C14 C 0.5936(5) 0.63413(15) 0.5044(5) 0.0494(9) Uani 1 1 d .
H14A H 0.6815 0.6321 0.4575 0.074 Uiso 1 1 calc R
H14B H 0.6471 0.6366 0.6178 0.074 Uiso 1 1 calc R
H14C H 0.5232 0.6632 0.4647 0.074 Uiso 1 1 calc R
C15 C 0.0434(6) 0.60017(17) 0.7906(6) 0.0602(12) Uani 1 1 d .
H15A H -0.0473 0.5875 0.8239 0.090 Uiso 1 1 calc R
H15B H -0.0050 0.6221 0.7015 0.090 Uiso 1 1 calc R
H15C H 0.1254 0.6183 0.8766 0.090 Uiso 1 1 calc R
C16 C 0.2027(5) 0.52491(17) 0.8770(4) 0.0535(11) Uani 1 1 d .
H16A H 0.2928 0.5416 0.9603 0.080 Uiso 1 1 calc R
H16B H 0.2499 0.4963 0.8418 0.080 Uiso 1 1 calc R
H16C H 0.1140 0.5142 0.9161 0.080 Uiso 1 1 calc R
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 '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
N1 Zr1 N2 76.17(9)
N1 Zr1 N3 96.43(10)
N2 Zr1 N3 94.42(10)
N1 Zr1 N4 95.93(10)
N2 Zr1 N4 91.98(10)
N3 Zr1 N4 167.13(10)
N1 Zr1 Cl1 94.07(7)
N2 Zr1 Cl1 169.91(7)
N3 Zr1 Cl1 84.00(8)
N4 Zr1 Cl1 91.58(7)
N1 Zr1 Cl2 168.70(7)
N2 Zr1 Cl2 92.66(7)
N3 Zr1 Cl2 85.99(7)
N4 Zr1 Cl2 82.57(7)
Cl1 Zr1 Cl2 97.16(3)
C5 N1 C1 114.0(2)
C5 N1 Zr1 117.17(18)
C1 N1 Zr1 128.8(2)
C9 N2 C12 114.3(2)
C9 N2 Zr1 117.30(18)
C12 N2 Zr1 128.4(2)
C14 N3 C13 110.4(3)
C14 N3 Zr1 112.4(2)
C13 N3 Zr1 116.7(2)
C15 N4 C16 110.8(3)
C15 N4 Zr1 113.2(2)
C16 N4 Zr1 117.8(2)
N1 C1 C2 112.7(3)
C3 C2 C1 110.7(3)
C4 C3 C2 110.2(3)
C5 C4 C6 117.6(3)
C5 C4 C3 120.9(3)
C6 C4 C3 121.5(3)
C4 C5 N1 124.3(3)
C4 C5 C9 120.8(3)
N1 C5 C9 114.8(2)
C7 C6 C4 121.8(3)
C6 C7 C8 121.3(3)
C7 C8 C9 117.9(3)
C7 C8 C10 122.0(3)
C9 C8 C10 120.0(3)
C8 C9 N2 125.1(3)
C8 C9 C5 120.5(3)
N2 C9 C5 114.4(2)
C8 C10 C11 109.6(3)
C12 C11 C10 110.8(3)
N2 C12 C11 113.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Zr1 N1 2.090(2)
Zr1 N2 2.092(2)
Zr1 N3 2.349(3)
Zr1 N4 2.358(3)
Zr1 Cl1 2.4806(8)
Zr1 Cl2 2.5353(8)
N1 C5 1.406(4)
N1 C1 1.471(4)
N2 C9 1.408(4)
N2 C12 1.467(4)
N3 C14 1.473(5)
N3 C13 1.479(5)
N4 C15 1.474(5)
N4 C16 1.476(5)
C1 C2 1.502(5)
C2 C3 1.502(5)
C3 C4 1.499(4)
C4 C5 1.390(4)
C4 C6 1.395(5)
C5 C9 1.408(4)
C6 C7 1.372(5)
C7 C8 1.391(5)
C8 C9 1.399(4)
C8 C10 1.495(4)
C10 C11 1.518(5)
C11 C12 1.499(5)
