#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/92/7019233.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_7019233
loop_
_publ_author_name
'Guard, Louise M.'
'Palma, Julio L.'
'Stratton, William P.'
'Allen, Laura J.'
'Brudvig, Gary W.'
'Crabtree, Robert H.'
'Batista, Victor S.'
'Hazari, Nilay'
_publ_section_title
;
 Synthesis and computational studies of Mg complexes supported by
 2,2':6,2''-terpyridine ligands.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8098
_journal_page_last               8110
_journal_paper_doi               10.1039/c2dt12426b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'Br2 Mg N3 C27 H35'
_chemical_formula_sum            'C27 H35 Br2 Mg N3'
_chemical_formula_weight         585.71
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      154
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_formula_units_Z            3
_cell_length_a                   12.5029(20)
_cell_length_b                   12.5029(20)
_cell_length_c                   15.991(3)
_cell_measurement_reflns_used    11997
_cell_measurement_temperature    223
_cell_measurement_theta_max      24.65
_cell_measurement_theta_min      3.17
_cell_volume                     2164.8(6)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 6.849
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Mercury275R CCD (SCX mini)'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13546
_diffrn_reflns_theta_full        24.40
_diffrn_reflns_theta_max         24.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             900.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.330
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 1019 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.038(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2392
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0424
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0424P)²+1.1135P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                2093
_reflns_number_total             2392
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c2dt12426b.txt
_cod_data_source_block           '_Compound5b'
_cod_original_cell_volume        2164.9(6)
_cod_original_formula_sum        'Br2 Mg N3 C27 H35'
_cod_database_code               7019233
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -Y,+X-Y,2/3+Z
3 -X+Y,-X,1/3+Z
4 +Y,+X,-Z
5 +X-Y,-Y,1/3-Z
6 -X,-X+Y,2/3-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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Br(1) Br 0.26164(6) 0.17783(5) 1.21309(3) 0.0611(2) Uani 1.00 6 d .
Mg(2) Mg 0.27942(17) 0.0000 1.1667 0.0312(4) Uani 1.00 3 d S
N(1) N 0.4482(3) 0.0000 1.1667 0.0307(10) Uani 1.00 3 d S
N(2) N 0.3634(3) 0.0716(4) 1.0467(2) 0.0353(8) Uani 1.00 6 d .
C(1) C 0.5192(4) 0.0335(4) 1.0980(2) 0.0318(9) Uani 1.00 6 d .
C(2) C 0.6280(4) 0.0298(4) 1.0951(3) 0.0367(10) Uani 1.00 6 d .
C(3) C 0.6696(5) 0.0000 1.1667 0.0401(14) Uani 1.00 3 d S
C(4) C 0.4688(4) 0.0727(4) 1.0275(3) 0.0323(10) Uani 1.00 6 d .
C(5) C 0.5259(4) 0.1158(5) 0.9525(3) 0.0389(11) Uani 1.00 6 d .
C(6) C 0.4790(4) 0.1618(5) 0.8929(3) 0.0459(12) Uani 1.00 6 d .
C(7) C 0.3720(5) 0.1608(5) 0.9141(3) 0.0465(12) Uani 1.00 6 d .
C(8) C 0.3177(4) 0.1155(5) 0.9901(3) 0.0475(12) Uani 1.00 6 d .
C(9) C 0.7928(6) 0.0000 1.1667 0.0531(20) Uani 1.00 3 d S
C(10) C 0.7754(17) -0.1018(18) 1.1003(10) 0.092(5) Uani 0.50 6 d P
C(11) C 0.8503(15) 0.018(2) 1.0863(9) 0.085(5) Uani 0.50 6 d P
C(12) C 0.8902(10) 0.1199(16) 1.1302(10) 0.086(5) Uani 0.50 6 d P
C(13) C 0.5422(6) 0.2123(7) 0.8092(3) 0.0679(18) Uani 1.00 6 d .
C(14) C 0.5647(10) 0.1182(10) 0.7658(4) 0.127(3) Uani 1.00 6 d .
C(15) C 0.4698(9) 0.2476(13) 0.7527(5) 0.165(6) Uani 1.00 6 d .
C(16) C 0.6670(8) 0.3204(9) 0.8266(6) 0.134(4) Uani 1.00 6 d .
H(5) H 0.5989 0.1145 0.9408 0.047 Uiso 1.00 6 calc R
H(2) H 0.6731 0.0475 1.0450 0.044 Uiso 1.00 6 calc R
H(8) H 0.2443 0.1156 1.0029 0.057 Uiso 1.00 6 calc R
H(7) H 0.3359 0.1912 0.8763 0.056 Uiso 1.00 6 calc R
H(14A) H 0.6156 0.0985 0.8010 0.153 Uiso 1.00 6 calc R
H(14B) H 0.6065 0.1518 0.7130 0.153 Uiso 1.00 6 calc R
H(14C) H 0.4863 0.0439 0.7553 0.153 Uiso 1.00 6 calc R
H(15A) H 0.5149 0.2806 0.7009 0.198 Uiso 1.00 6 calc R
H(15B) H 0.4572 0.3098 0.7798 0.198 Uiso 1.00 6 calc R
H(15C) H 0.3905 0.1754 0.7408 0.198 Uiso 1.00 6 calc R
H(16A) H 0.7092 0.3552 0.7742 0.161 Uiso 1.00 6 calc R
H(16B) H 0.7146 0.2937 0.8595 0.161 Uiso 1.00 6 calc R
H(16C) H 0.6582 0.3824 0.8573 0.161 Uiso 1.00 6 calc R
H(10A) H 0.8463 -0.1138 1.1023 0.111 Uiso 0.50 6 calc R
H(10B) H 0.7682 -0.0749 1.0448 0.111 Uiso 0.50 6 calc R
H(10C) H 0.7012 -0.1790 1.1134 0.111 Uiso 0.50 6 calc R
H(11A) H 0.8805 0.1027 1.0682 0.102 Uiso 0.50 6 calc R
H(11B) H 0.7905 -0.0381 1.0462 0.102 Uiso 0.50 6 calc R
H(11C) H 0.9188 0.0029 1.0902 0.102 Uiso 0.50 6 calc R
H(12A) H 0.9035 0.1872 1.1669 0.103 Uiso 0.50 6 calc R
H(12B) H 0.8637 0.1318 1.0758 0.103 Uiso 0.50 6 calc R
H(12C) H 0.9667 0.1182 1.1244 0.103 Uiso 0.50 6 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.290 2.459
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Mg Mg 0.049 0.036
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 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_publ_flag
Br(1) Mg(2) N(1) 122.88(4) yes
Br(1) Mg(2) N(2) 97.97(13) yes
N(1) Mg(2) N(2) 73.79(14) yes
Mg(2) N(1) C(1) 120.4(3) yes
Mg(2) N(2) C(4) 118.5(3) yes
Mg(2) N(2) C(8) 123.9(4) yes
C(4) N(2) C(8) 117.6(4) yes
N(1) C(1) C(2) 121.7(4) yes
N(1) C(1) C(4) 113.6(4) yes
C(2) C(1) C(4) 124.7(4) yes
C(1) C(2) C(3) 119.3(4) yes
C(2) C(3) C(9) 120.7(3) yes
N(2) C(4) C(1) 113.4(4) yes
N(2) C(4) C(5) 121.4(5) yes
C(1) C(4) C(5) 124.9(5) yes
C(4) C(5) C(6) 121.6(5) yes
C(5) C(6) C(7) 116.0(4) yes
C(5) C(6) C(13) 122.5(6) yes
C(7) C(6) C(13) 121.5(6) yes
C(6) C(7) C(8) 120.1(6) yes
N(2) C(8) C(7) 123.3(6) yes
C(3) C(9) C(10) 105.3(8) yes
C(3) C(9) C(11) 114.9(9) yes
C(3) C(9) C(12) 108.3(8) yes
C(10) C(9) C(11) 52.1(11) yes
C(10) C(9) C(12) 105.0(9) yes
C(11) C(9) C(12) 53.1(11) yes
C(9) C(10) C(11) 58.0(11) yes
C(9) C(11) C(10) 69.9(11) yes
C(9) C(11) C(12) 66.0(11) yes
C(10) C(11) C(12) 135.6(15) yes
C(9) C(12) C(11) 61.0(9) yes
C(6) C(13) C(14) 110.0(6) yes
C(6) C(13) C(15) 112.9(6) yes
C(6) C(13) C(16) 107.6(5) yes
C(14) C(13) C(15) 109.2(7) yes
C(14) C(13) C(16) 105.9(8) yes
C(15) C(13) C(16) 111.0(8) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Br(1) Mg(2) 2.4571(14) yes
Mg(2) N(1) 2.110(4) yes
Mg(2) N(2) 2.156(3) yes
N(1) C(1) 1.342(4) yes
N(2) C(4) 1.347(7) yes
N(2) C(8) 1.326(7) yes
C(1) C(2) 1.384(8) yes
C(1) C(4) 1.489(7) yes
C(2) C(3) 1.385(6) yes
C(3) C(9) 1.540(10) yes
C(4) C(5) 1.362(6) yes
C(5) C(6) 1.385(8) yes
C(6) C(7) 1.375(9) yes
C(6) C(13) 1.522(7) yes
C(7) C(8) 1.370(6) yes
C(9) C(10) 1.59(2) yes
C(9) C(11) 1.434(16) yes
C(9) C(12) 1.498(14) yes
C(13) C(14) 1.508(16) yes
C(13) C(15) 1.493(16) yes
C(13) C(16) 1.493(9) yes
C(2) H(2) 0.940 yes
C(5) H(5) 0.940 yes
C(7) H(7) 0.940 yes
C(8) H(8) 0.940 yes
C(10) H(10A) 0.970 yes
C(10) H(10B) 0.970 yes
C(10) H(10C) 0.970 yes
C(11) H(10B) 1.288 yes
C(11) H(11A) 0.970 yes
C(11) H(11B) 0.970 yes
C(11) H(11C) 0.970 yes
C(12) H(12A) 0.970 yes
C(12) H(12B) 0.970 yes
C(12) H(12C) 0.970 yes
C(14) H(14A) 0.970 yes
C(14) H(14B) 0.970 yes
C(14) H(14C) 0.970 yes
C(15) H(15A) 0.970 yes
C(15) H(15B) 0.970 yes
C(15) H(15C) 0.970 yes
C(16) H(16A) 0.970 yes
C(16) H(16B) 0.970 yes
C(16) H(16C) 0.970 yes
H(10B) H(11B) 0.402 yes
H(11A) H(12B) 0.516 yes
