#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:46:06 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195074 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/24/7042436.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_7042436
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         'C4 H10 Cl2 Mg O2'
_chemical_formula_sum            'C4 H10 Cl2 Mg O2'
_chemical_formula_weight         185.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-01-15 deposited with the CCDC.
2017-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.5400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.2117(4)
_cell_length_b                   13.5279(4)
_cell_length_c                   13.0025(4)
_cell_measurement_reflns_used    9749
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      37.52
_cell_measurement_theta_min      2.74
_cell_volume                     1568.41(10)
_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.3.2g (Brandenburg, 2011)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '62mm x 62mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Bruker KAPPA APEX II DUO CCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'curved graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0078
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51157
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.490
_diffrn_reflns_theta_min         2.736
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.093
_refine_diff_density_max         0.629
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         3854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0179
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0256P)²+0.8070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0504
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3588
_reflns_number_total             3854
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00193b2.cif
_cod_data_source_block           dme
_cod_depositor_comments
'Adding full bibliography for 7042435--7042437.cif.'
_cod_database_code               7042436
_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   0.893
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.88255(7) 0.55320(5) 0.10321(6) 0.01777(11) Uani 1 1 d . .
H1A H 0.8453 0.4940 0.0615 0.027 Uiso 1 1 calc R U
H1B H 0.9583 0.5855 0.0737 0.027 Uiso 1 1 calc R U
H1C H 0.9275 0.5344 0.1771 0.027 Uiso 1 1 calc R U
C2 C 0.80703(7) 0.70924(5) 0.15909(5) 0.01565(10) Uani 1 1 d . .
H2A H 0.8945 0.7389 0.1393 0.019 Uiso 1 1 calc R U
H2B H 0.8349 0.6950 0.2362 0.019 Uiso 1 1 calc R U
C3 C 0.67476(8) 0.77791(5) 0.13146(6) 0.01676(11) Uani 1 1 d . .
H3A H 0.6934 0.8369 0.1780 0.020 Uiso 1 1 calc R U
H3B H 0.6569 0.8000 0.0567 0.020 Uiso 1 1 calc R U
C4 C 0.41255(8) 0.78234(5) 0.11487(5) 0.01664(11) Uani 1 1 d . .
H4A H 0.3275 0.7440 0.1260 0.025 Uiso 1 1 calc R U
H4B H 0.4238 0.8429 0.1576 0.025 Uiso 1 1 calc R U
H4C H 0.3946 0.7997 0.0395 0.025 Uiso 1 1 calc R U
Mg1 Mg 0.54768(2) 0.56887(2) 0.12297(2) 0.00952(4) Uani 1 1 d . .
Cl1 Cl 0.57864(2) 0.39885(2) 0.06891(2) 0.01142(3) Uani 1 1 d . .
Cl2 Cl 0.31652(2) 0.54382(2) 0.18331(2) 0.01109(3) Uani 1 1 d . .
O1 O 0.76041(5) 0.62014(3) 0.09928(4) 0.01247(8) Uani 1 1 d . .
O2 O 0.54713(5) 0.72439(3) 0.14646(4) 0.01214(7) 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'
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'
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
O1 C1 H1A 109.5 . .
O1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
O1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
O1 C2 C3 105.92(5) . .
O1 C2 H2A 110.6 . .
C3 C2 H2A 110.6 . .
O1 C2 H2B 110.6 . .
C3 C2 H2B 110.6 . .
H2A C2 H2B 108.7 . .
O2 C3 C2 107.37(5) . .
O2 C3 H3A 110.2 . .
C2 C3 H3A 110.2 . .
O2 C3 H3B 110.2 . .
C2 C3 H3B 110.2 . .
H3A C3 H3B 108.5 . .
O2 C4 H4A 109.5 . .
O2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
O2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O2 Mg1 O1 74.879(19) . .
O2 Mg1 Cl1 167.899(17) . .
O1 Mg1 Cl1 94.887(15) . .
O2 Mg1 Cl2 93.255(15) . .
O1 Mg1 Cl2 165.677(17) . .
Cl1 Mg1 Cl2 97.729(9) . .
O2 Mg1 Cl1 87.332(15) . 5_665
O1 Mg1 Cl1 90.753(15) . 5_665
Cl1 Mg1 Cl1 86.349(8) . 5_665
Cl2 Mg1 Cl1 96.775(9) . 5_665
O2 Mg1 Cl2 90.452(15) . 2_655
O1 Mg1 Cl2 86.900(15) . 2_655
Cl1 Mg1 Cl2 95.499(9) . 2_655
Cl2 Mg1 Cl2 85.174(8) . 2_655
Cl1 Mg1 Cl2 177.125(11) 5_665 2_655
O2 Mg1 Mg1 128.942(17) . 5_665
O1 Mg1 Mg1 93.825(15) . 5_665
Cl1 Mg1 Mg1 43.930(6) . 5_665
Cl2 Mg1 Mg1 99.957(10) . 5_665
Cl1 Mg1 Mg1 42.419(6) 5_665 5_665
Cl2 Mg1 Mg1 139.384(11) 2_655 5_665
O2 Mg1 Mg1 81.908(14) . 2_655
O1 Mg1 Mg1 124.247(16) . 2_655
Cl1 Mg1 Mg1 109.559(6) . 2_655
Cl2 Mg1 Mg1 44.376(6) . 2_655
Cl1 Mg1 Mg1 138.346(11) 5_665 2_655
Cl2 Mg1 Mg1 42.901(6) 2_655 2_655
Mg1 Mg1 Mg1 138.220(9) 5_665 2_655
Mg1 Cl1 Mg1 93.651(8) . 5_665
Mg1 Cl2 Mg1 92.723(8) . 2_655
C1 O1 C2 112.58(5) . .
C1 O1 Mg1 121.36(4) . .
C2 O1 Mg1 110.37(4) . .
C3 O2 C4 111.31(5) . .
C3 O2 Mg1 116.62(4) . .
C4 O2 Mg1 122.13(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.4353(8) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 O1 1.4402(8) .
C2 C3 1.5023(10) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 O2 1.4350(8) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 O2 1.4369(8) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
Mg1 O2 2.1261(5) .
Mg1 O1 2.1723(5) .
Mg1 Cl1 2.4426(3) .
Mg1 Cl2 2.4705(3) .
Mg1 Cl1 2.5123(3) 5_665
Mg1 Cl2 2.5382(3) 2_655
Mg1 Mg1 3.6138(4) 5_665
Mg1 Mg1 3.6251(4) 2_655
Cl1 Mg1 2.5122(3) 5_665
Cl2 Mg1 2.5381(3) 2_655
