#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:46:06 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/24/7042435.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_7042435
loop_
_publ_author_name
'Nissinen, V. H.'
'Koshevoy, I. O.'
'Pakkanen, T. T.'
_publ_section_title
;
 Crystalline magnesium chloride-electron donor complexes: new support
 materials for Ziegler-Natta catalysts.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4452
_journal_page_last               4460
_journal_paper_doi               10.1039/c7dt00193b
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C12 H32 Cl2 Mg N4'
_chemical_formula_sum            'C12 H32 Cl2 Mg N4'
_chemical_formula_weight         327.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-15 deposited with the CCDC.
2017-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                84.028(2)
_cell_angle_beta                 84.0440(10)
_cell_angle_gamma                84.4590(10)
_cell_formula_units_Z            1
_cell_length_a                   6.7256(4)
_cell_length_b                   7.9186(5)
_cell_length_c                   8.2724(5)
_cell_measurement_reflns_used    7937
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.97
_cell_measurement_theta_min      2.60
_cell_volume                     434.17(5)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'Diamond v.4.03 (Brandenburg, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device       '62mm x 62mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II CCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11005
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.027
_diffrn_reflns_theta_min         2.596
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       block
_exptl_crystal_F_000             178
_exptl_crystal_size_max          0.803
_exptl_crystal_size_mid          0.612
_exptl_crystal_size_min          0.536
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0307P)²+0.0603P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3252
_reflns_number_total             3531
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00193b2.cif
_cod_data_source_block           deeda
_cod_depositor_comments
'Adding full bibliography for 7042435--7042437.cif.'
_cod_database_code               7042435
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.737
_shelx_estimated_absorpt_t_max   0.812
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.23593(11) 0.89752(9) 0.16573(9) 0.02568(13) Uani 1 1 d . . .
H1A H 0.2375 0.9899 0.2356 0.039 Uiso 1 1 calc R U .
H1B H 0.3556 0.8961 0.0873 0.039 Uiso 1 1 calc R U .
H1C H 0.1155 0.9157 0.1067 0.039 Uiso 1 1 calc R U .
C2 C 0.23467(10) 0.72914(8) 0.26991(8) 0.02063(11) Uani 1 1 d . . .
H2A H 0.3552 0.7124 0.3310 0.025 Uiso 1 1 calc R U .
H2B H 0.1150 0.7320 0.3504 0.025 Uiso 1 1 calc R U .
C3 C 0.19708(9) 0.42587(8) 0.27831(8) 0.01994(11) Uani 1 1 d . . .
H3A H 0.1370 0.3459 0.2170 0.024 Uiso 1 1 calc R U .
H3B H 0.1010 0.4532 0.3729 0.024 Uiso 1 1 calc R U .
C4 C 0.39140(10) 0.34161(8) 0.33860(7) 0.02043(11) Uani 1 1 d . . .
H4A H 0.4533 0.4219 0.3982 0.025 Uiso 1 1 calc R U .
H4B H 0.3634 0.2399 0.4148 0.025 Uiso 1 1 calc R U .
C5 C 0.73323(9) 0.23176(8) 0.24848(8) 0.02027(11) Uani 1 1 d . . .
H5A H 0.7805 0.3208 0.3071 0.024 Uiso 1 1 calc R U .
H5B H 0.8264 0.2185 0.1489 0.024 Uiso 1 1 calc R U .
C6 C 0.74336(11) 0.06440(9) 0.35695(9) 0.02553(13) Uani 1 1 d . . .
H6A H 0.8815 0.0342 0.3842 0.038 Uiso 1 1 calc R U .
H6B H 0.6546 0.0768 0.4575 0.038 Uiso 1 1 calc R U .
H6C H 0.7006 -0.0257 0.2990 0.038 Uiso 1 1 calc R U .
N1 N 0.23224(7) 0.58383(7) 0.17153(6) 0.01607(9) Uani 1 1 d . . .
H1N1 H 0.1312 0.6063 0.1191 0.019 Uiso 1 1 d R U .
N2 N 0.53099(7) 0.29084(6) 0.19895(6) 0.01611(9) Uani 1 1 d . . .
H1N2 H 0.4848 0.2054 0.1647 0.019 Uiso 1 1 d R U .
Mg1 Mg 0.5000 0.5000 0.0000 0.01388(6) Uani 1 2 d S . P
Cl1 Cl 0.73333(2) 0.66581(2) 0.12273(2) 0.02048(4) Uani 1 1 d . . .
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'
Mg Mg 0.0486 0.0363 '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'
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 C1 H1A 109.5 . .
C2 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C2 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 C1 112.22(5) . .
N1 C2 H2A 109.2 . .
C1 C2 H2A 109.2 . .
N1 C2 H2B 109.2 . .
C1 C2 H2B 109.2 . .
H2A C2 H2B 107.9 . .
N1 C3 C4 111.04(5) . .
N1 C3 H3A 109.4 . .
C4 C3 H3A 109.4 . .
N1 C3 H3B 109.4 . .
C4 C3 H3B 109.4 . .
H3A C3 H3B 108.0 . .
N2 C4 C3 109.83(5) . .
N2 C4 H4A 109.7 . .
C3 C4 H4A 109.7 . .
N2 C4 H4B 109.7 . .
C3 C4 H4B 109.7 . .
H4A C4 H4B 108.2 . .
N2 C5 C6 114.48(5) . .
N2 C5 H5A 108.6 . .
C6 C5 H5A 108.6 . .
N2 C5 H5B 108.6 . .
C6 C5 H5B 108.6 . .
H5A C5 H5B 107.6 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C3 N1 C2 110.65(5) . .
C3 N1 Mg1 102.55(3) . .
C2 N1 Mg1 121.82(4) . .
C3 N1 H1N1 106.2 . .
C2 N1 H1N1 105.4 . .
Mg1 N1 H1N1 109.3 . .
C4 N2 C5 111.85(5) . .
C4 N2 Mg1 106.53(4) . .
C5 N2 Mg1 119.06(4) . .
C4 N2 H1N2 106.6 . .
C5 N2 H1N2 106.8 . .
Mg1 N2 H1N2 105.2 . .
N2 Mg1 N2 180.0 2_665 .
N2 Mg1 N1 98.620(18) 2_665 .
N2 Mg1 N1 81.380(19) . .
N2 Mg1 N1 81.380(19) 2_665 2_665
N2 Mg1 N1 98.620(19) . 2_665
N1 Mg1 N1 180.0 . 2_665
N2 Mg1 Cl1 89.365(14) 2_665 .
N2 Mg1 Cl1 90.635(14) . .
N1 Mg1 Cl1 93.411(14) . .
N1 Mg1 Cl1 86.589(14) 2_665 .
N2 Mg1 Cl1 90.635(14) 2_665 2_665
N2 Mg1 Cl1 89.365(14) . 2_665
N1 Mg1 Cl1 86.589(14) . 2_665
N1 Mg1 Cl1 93.411(14) 2_665 2_665
Cl1 Mg1 Cl1 180.0 . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.5107(9) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 N1 1.4791(8) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 N1 1.4780(8) .
C3 C4 1.5165(9) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 N2 1.4753(8) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 N2 1.4798(8) .
C5 C6 1.5211(9) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
N1 Mg1 2.2654(5) .
N1 H1N1 0.8386 .
N2 Mg1 2.2209(5) .
N2 H1N2 0.8565 .
Mg1 N2 2.2209(5) 2_665
Mg1 N1 2.2654(5) 2_665
Mg1 Cl1 2.49463(16) .
Mg1 Cl1 2.49464(17) 2_665
