#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:10:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178551 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/58/4065837.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_4065837
loop_
_publ_author_name
'Bonello, Owen'
'Jones, Cameron'
'Stasch, Andreas'
'Woodul, William D.'
_publ_section_title
;
 Group 2 and 12 Metal Gallyl Complexes Containing Unsupported Ga−M
 Covalent Bonds (M = Mg, Ca, Sr, Ba, Zn, Cd)†
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              4914
_journal_paper_doi               10.1021/om1001606
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C64 H104 Ga2 N8 Sr'
_chemical_formula_weight         1212.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 131.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.407(6)
_cell_length_b                   14.031(3)
_cell_length_c                   21.729(4)
_cell_measurement_temperature    123(2)
_cell_volume                     6709(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0777
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11084
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.673
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5872
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1003P)²+21.6242P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1678
_refine_ls_wR_factor_ref         0.1942
_reflns_number_gt                3863
_reflns_number_total             5872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1001606_si_002.cif
_cod_data_source_block           compound9
_cod_original_cell_volume        6709(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4065837
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sr1 Sr 0.0000 0.0000 0.0000 0.0349(3) Uani 1 2 d S
Ga1 Ga 0.11121(3) 0.16008(4) 0.09378(4) 0.0350(2) Uani 1 1 d .
N1 N 0.1478(2) 0.2526(3) 0.1806(3) 0.0379(12) Uani 1 1 d .
C1 C 0.1878(3) 0.3120(5) 0.1850(4) 0.0538(19) Uani 1 1 d .
H1 H 0.2096 0.3612 0.2249 0.065 Uiso 1 1 calc R
N2 N 0.1611(2) 0.2208(3) 0.0765(3) 0.0382(12) Uani 1 1 d .
C2 C 0.1938(3) 0.2960(5) 0.1297(4) 0.0536(19) Uani 1 1 d .
H2 H 0.2192 0.3344 0.1274 0.064 Uiso 1 1 calc R
N3 N 0.0005(3) 0.0050(5) 0.1227(5) 0.077(2) Uani 1 1 d .
C3 C 0.1443(3) 0.2613(5) 0.2434(5) 0.054(2) Uani 1 1 d .
N4 N 0.0742(3) -0.1407(5) 0.1064(4) 0.075(2) Uani 1 1 d .
C4 C 0.0981(4) 0.3105(7) 0.2286(6) 0.076(3) Uani 1 1 d .
C5 C 0.0956(5) 0.3159(9) 0.2930(8) 0.105(4) Uani 1 1 d .
H5 H 0.0649 0.3518 0.2857 0.125 Uiso 1 1 calc R
C6 C 0.1382(6) 0.2685(8) 0.3633(8) 0.098(3) Uani 1 1 d U
H6 H 0.1355 0.2706 0.4045 0.117 Uiso 1 1 calc R
C7 C 0.1833(6) 0.2196(8) 0.3798(6) 0.094(3) Uani 1 1 d .
H7 H 0.2120 0.1885 0.4313 0.113 Uiso 1 1 calc R
C8 C 0.1884(4) 0.2140(6) 0.3192(5) 0.070(3) Uani 1 1 d .
C9 C 0.0522(4) 0.3596(8) 0.1486(7) 0.087(3) Uani 1 1 d .
H9 H 0.0478 0.3197 0.1068 0.105 Uiso 1 1 calc R
C10 C -0.0120(5) 0.3659(9) 0.1193(8) 0.126(4) Uani 1 1 d U
H10A H -0.0099 0.3994 0.1607 0.188 Uiso 1 1 calc R
H10B H -0.0280 0.3015 0.1115 0.188 Uiso 1 1 calc R
H10C H -0.0389 0.4008 0.0671 0.188 Uiso 1 1 calc R
C11 C 0.0700(5) 0.4544(10) 0.1431(8) 0.127(4) Uani 1 1 d .
H11A H 0.0813 0.4941 0.1885 0.191 Uiso 1 1 calc R
H11B H 0.0358 0.4839 0.0906 0.191 Uiso 1 1 calc R
H11C H 0.1048 0.4488 0.1464 0.191 Uiso 1 1 calc R
C12 C 0.2421(5) 0.1606(6) 0.3390(5) 0.079(3) Uani 1 1 d .
H12 H 0.2475 0.1852 0.3010 0.094 Uiso 1 1 calc R
C13 C 0.2279(5) 0.0519(7) 0.3215(7) 0.106(3) Uani 1 1 d .
H13A H 0.2179 0.0271 0.3534 0.159 Uiso 1 1 calc R
H13B H 0.2636 0.0183 0.3375 0.159 Uiso 1 1 calc R
H13C H 0.1934 0.0420 0.2628 0.159 Uiso 1 1 calc R
C14 C 0.3027(5) 0.1704(8) 0.4260(7) 0.121(4) Uani 1 1 d .
H14A H 0.3146 0.2376 0.4377 0.182 Uiso 1 1 calc R
H14B H 0.3336 0.1335 0.4317 0.182 Uiso 1 1 calc R
H14C H 0.2989 0.1463 0.4648 0.182 Uiso 1 1 calc R
C15 C 0.1670(3) 0.2007(4) 0.0176(4) 0.0348(14) Uani 1 1 d .
C16 C 0.1434(3) 0.2627(5) -0.0477(4) 0.0463(17) Uani 1 1 d .
C17 C 0.1520(3) 0.2409(5) -0.1026(4) 0.0486(17) Uani 1 1 d .
H17 H 0.1363 0.2826 -0.1473 0.058 Uiso 1 1 calc R
C18 C 0.1825(3) 0.1609(5) -0.0926(4) 0.0460(17) Uani 1 1 d .
H18 H 0.1885 0.1480 -0.1297 0.055 Uiso 1 1 calc R
C19 C 0.2049(3) 0.0985(5) -0.0291(4) 0.0491(17) Uani 1 1 d .
H19 H 0.2250 0.0419 -0.0236 0.059 Uiso 1 1 calc R
C20 C 0.1979(3) 0.1180(5) 0.0271(4) 0.0391(15) Uani 1 1 d .
C21 C 0.1074(5) 0.3504(5) -0.0611(6) 0.076(3) Uani 1 1 d .
H21 H 0.1070 0.3568 -0.0156 0.092 Uiso 1 1 calc R
C22 C 0.1291(5) 0.4408(7) -0.0706(8) 0.112(3) Uani 1 1 d U
H22A H 0.1206 0.4392 -0.1225 0.168 Uiso 1 1 calc R
H22B H 0.1730 0.4473 -0.0247 0.168 Uiso 1 1 calc R
H22C H 0.1081 0.4951 -0.0708 0.168 Uiso 1 1 calc R
C23 C 0.0399(6) 0.3449(10) -0.1475(10) 0.154(5) Uani 1 1 d U
H23A H 0.0266 0.4086 -0.1720 0.231 Uiso 1 1 calc R
H23B H 0.0128 0.3208 -0.1395 0.231 Uiso 1 1 calc R
H23C H 0.0386 0.3018 -0.1841 0.231 Uiso 1 1 calc R
C24 C 0.2242(3) 0.0497(5) 0.0982(4) 0.0540(19) Uani 1 1 d .
H24 H 0.1931 0.0433 0.1035 0.065 Uiso 1 1 calc R
C25 C 0.2814(4) 0.0921(8) 0.1798(5) 0.084(3) Uani 1 1 d .
H25A H 0.3130 0.1008 0.1770 0.126 Uiso 1 1 calc R
H25B H 0.2961 0.0486 0.2250 0.126 Uiso 1 1 calc R
H25C H 0.2714 0.1538 0.1893 0.126 Uiso 1 1 calc R
C26 C 0.2365(5) -0.0509(6) 0.0850(6) 0.084(3) Uani 1 1 d .
H26A H 0.2003 -0.0746 0.0311 0.126 Uiso 1 1 calc R
H26B H 0.2462 -0.0931 0.1282 0.126 Uiso 1 1 calc R
H26C H 0.2708 -0.0492 0.0870 0.126 Uiso 1 1 calc R
C27 C 0.0229(9) -0.0923(13) 0.1626(11) 0.178(6) Uani 1 1 d U
H27A H 0.0320 -0.0899 0.2154 0.214 Uiso 1 1 calc R
H27B H -0.0105 -0.1387 0.1267 0.214 Uiso 1 1 calc R
C28 C 0.0780(6) -0.1288(9) 0.1794(6) 0.120(4) Uani 1 1 d .
H28A H 0.0886 -0.1915 0.2068 0.145 Uiso 1 1 calc R
H28B H 0.1121 -0.0850 0.2191 0.145 Uiso 1 1 calc R
C29 C -0.0570(5) -0.0052(8) 0.0987(7) 0.101(3) Uani 1 1 d U
H29A H -0.0520 -0.0158 0.1475 0.151 Uiso 1 1 calc R
H29B H -0.0782 -0.0597 0.0614 0.151 Uiso 1 1 calc R
H29C H -0.0809 0.0528 0.0705 0.151 Uiso 1 1 calc R
C30 C 0.0336(5) 0.0801(8) 0.1809(6) 0.102(3) Uani 1 1 d U
H30A H 0.0126 0.1407 0.1549 0.153 Uiso 1 1 calc R
H30B H 0.0746 0.0832 0.2001 0.153 Uiso 1 1 calc R
H30C H 0.0364 0.0681 0.2277 0.153 Uiso 1 1 calc R
C31 C 0.1361(5) -0.1317(8) 0.1365(7) 0.109(3) Uani 1 1 d U
H31A H 0.1611 -0.1852 0.1731 0.163 Uiso 1 1 calc R
H31B H 0.1542 -0.0717 0.1666 0.163 Uiso 1 1 calc R
H31C H 0.1341 -0.1323 0.0896 0.163 Uiso 1 1 calc R
C32 C 0.0548(6) -0.2395(8) 0.0751(8) 0.126(4) Uani 1 1 d U
H32A H 0.0480 -0.2462 0.0247 0.189 Uiso 1 1 calc R
H32B H 0.0169 -0.2535 0.0631 0.189 Uiso 1 1 calc R
H32C H 0.0864 -0.2842 0.1167 0.189 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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sr Sr -1.5307 3.2498 '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
N3 Sr1 N3 180.0(3) 5 .
N3 Sr1 N4 72.4(2) 5 5
N3 Sr1 N4 107.6(2) . 5
N3 Sr1 N4 107.6(2) 5 .
N3 Sr1 N4 72.4(2) . .
N4 Sr1 N4 180.0(4) 5 .
N3 Sr1 Ga1 91.05(13) 5 5
N3 Sr1 Ga1 88.95(13) . 5
N4 Sr1 Ga1 93.53(15) 5 5
N4 Sr1 Ga1 86.47(15) . 5
N3 Sr1 Ga1 88.95(13) 5 .
N3 Sr1 Ga1 91.05(13) . .
N4 Sr1 Ga1 86.47(15) 5 .
N4 Sr1 Ga1 93.53(15) . .
Ga1 Sr1 Ga1 180.00(2) 5 .
N1 Ga1 N2 83.69(19) . .
N1 Ga1 Sr1 137.68(14) . .
N2 Ga1 Sr1 137.92(14) . .
C1 N1 C3 118.2(5) . .
C1 N1 Ga1 111.7(4) . .
C3 N1 Ga1 129.8(4) . .
C2 C1 N1 116.4(6) . .
C2 N2 C15 118.1(5) . .
C2 N2 Ga1 111.7(4) . .
C15 N2 Ga1 130.1(4) . .
C1 C2 N2 116.5(5) . .
C29 N3 C30 110.4(7) . .
C29 N3 C27 94.5(9) . .
C30 N3 C27 112.2(10) . .
C29 N3 Sr1 114.9(6) . .
C30 N3 Sr1 117.2(5) . .
C27 N3 Sr1 105.2(7) . .
C4 C3 C8 121.1(7) . .
C4 C3 N1 120.5(8) . .
C8 C3 N1 118.4(6) . .
C31 N4 C32 105.7(8) . .
C31 N4 C28 108.3(8) . .
C32 N4 C28 108.7(8) . .
C31 N4 Sr1 112.0(6) . .
C32 N4 Sr1 116.3(6) . .
C28 N4 Sr1 105.7(6) . .
C3 C4 C5 118.7(10) . .
C3 C4 C9 120.2(7) . .
C5 C4 C9 121.0(9) . .
C6 C5 C4 117.7(10) . .
C7 C6 C5 125.3(11) . .
C6 C7 C8 119.0(11) . .
C3 C8 C7 118.2(9) . .
C3 C8 C12 122.4(6) . .
C7 C8 C12 119.4(9) . .
C11 C9 C4 114.9(9) . .
C11 C9 C10 108.7(9) . .
C4 C9 C10 115.0(9) . .
C14 C12 C8 116.5(8) . .
C14 C12 C13 107.1(8) . .
C8 C12 C13 110.5(8) . .
C16 C15 C20 120.3(5) . .
C16 C15 N2 120.7(5) . .
C20 C15 N2 118.9(5) . .
C15 C16 C17 118.5(6) . .
C15 C16 C21 121.1(6) . .
C17 C16 C21 120.4(6) . .
C18 C17 C16 120.9(6) . .
C17 C18 C19 120.7(6) . .
C18 C19 C20 120.2(6) . .
C19 C20 C15 119.4(6) . .
C19 C20 C24 119.7(6) . .
C15 C20 C24 120.9(5) . .
C22 C21 C16 114.0(8) . .
C22 C21 C23 101.0(8) . .
C16 C21 C23 110.7(8) . .
C20 C24 C26 114.4(6) . .
C20 C24 C25 110.9(6) . .
C26 C24 C25 111.1(7) . .
C28 C27 N3 115.9(13) . .
C27 C28 N4 117.7(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sr1 N3 2.656(6) 5
Sr1 N3 2.656(6) .
Sr1 N4 2.704(7) 5
Sr1 N4 2.704(7) .
Sr1 Ga1 3.3241(11) 5
Sr1 Ga1 3.3241(11) .
Ga1 N1 1.925(5) .
Ga1 N2 1.938(4) .
N1 C1 1.391(7) .
N1 C3 1.442(8) .
C1 C2 1.344(9) .
N2 C2 1.377(8) .
N2 C15 1.431(7) .
N3 C29 1.410(11) .
N3 C30 1.422(11) .
N3 C27 1.515(17) .
C3 C4 1.357(11) .
C3 C8 1.415(11) .
N4 C31 1.476(12) .
N4 C32 1.482(12) .
N4 C28 1.522(13) .
C4 C5 1.452(12) .
C4 C9 1.484(13) .
C5 C6 1.345(14) .
C6 C7 1.316(14) .
C7 C8 1.423(11) .
C8 C12 1.529(13) .
C9 C11 1.464(14) .
C9 C10 1.543(13) .
C12 C14 1.516(13) .
C12 C13 1.560(12) .
C15 C16 1.394(8) .
C15 C20 1.402(9) .
C16 C17 1.410(8) .
C16 C21 1.519(10) .
C17 C18 1.361(9) .
C18 C19 1.379(9) .
C19 C20 1.391(8) .
C20 C24 1.522(9) .
C21 C22 1.495(12) .
C21 C23 1.589(16) .
C24 C26 1.531(11) .
C24 C25 1.538(11) .
C27 C28 1.496(19) .
