#------------------------------------------------------------------------------
#$Date: 2019-11-24 11:54:30 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237854 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/88/4088849.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_4088849
loop_
_publ_author_name
'Klimovica, Kristine'
'Kirschbaum, Kristin'
'Daugulis, Olafs'
_publ_section_title
;
 Synthesis and Properties of "Sandwich" Diimine-Coinage Metal
 Ethylene Complexes.
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              2938
_journal_page_last               2943
_journal_paper_doi               10.1021/acs.organomet.6b00487
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C47 H46 Ag B Cl8 F4 N2'
_chemical_formula_weight         1117.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 94.631(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.982(4)
_cell_length_b                   23.133(8)
_cell_length_c                   17.482(9)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.864
_cell_measurement_theta_min      2.655
_cell_volume                     4830(3)
_computing_cell_refinement       'SAINT Apex2'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT, Apex2'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX2 DUO'
_diffrn_measurement_method       /w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17154
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.918
_diffrn_reflns_theta_min         1.463
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6067
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       rod
_exptl_crystal_F_000             2264
_refine_diff_density_max         1.945
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         5851
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0489
_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)+(0.0662P)²+20.8996P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4943
_reflns_number_total             5851
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om6b00487_si_002.cif
_cod_data_source_block           Ag
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               4088849
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.5000 0.17357(2) 0.5000 0.02638(11) Uani 1 2 d S T P . .
N4 N 0.58170(19) 0.25172(12) 0.45326(13) 0.0234(5) Uani 1 1 d . . . . .
C1 C 0.5470(4) 0.08135(19) 0.4813(3) 0.0604(12) Uani 1 1 d . . . . .
H1A H 0.5394 0.0675 0.4276 0.072 Uiso 1 1 calc R U . . .
H1B H 0.6159 0.0675 0.5107 0.072 Uiso 1 1 calc R U . . .
C2 C 0.5955(4) 0.35832(16) 0.4527(2) 0.0380(8) Uani 1 1 d . . . . .
H2A H 0.649(4) 0.353(2) 0.415(3) 0.057 Uiso 1 1 d . U . . .
H2B H 0.532(4) 0.383(2) 0.431(3) 0.057 Uiso 1 1 d . U . . .
H2C H 0.629(4) 0.373(2) 0.492(3) 0.057 Uiso 1 1 d . U . . .
C3 C 0.5491(2) 0.30109(15) 0.47509(16) 0.0269(6) Uani 1 1 d . . . . .
C4 C 0.6621(2) 0.20907(14) 0.34133(16) 0.0258(6) Uani 1 1 d . . . . .
C5 C 0.6756(2) 0.24304(14) 0.40990(16) 0.0262(6) Uani 1 1 d . . . . .
C6 C 0.7797(3) 0.26043(17) 0.44040(19) 0.0349(7) Uani 1 1 d . . . . .
H6A H 0.7859 0.2846 0.4845 0.042 Uiso 1 1 calc R U . . .
C7 C 0.8768(3) 0.2428(2) 0.4069(2) 0.0433(9) Uani 1 1 d . . . . .
H7A H 0.9483 0.2554 0.4279 0.052 Uiso 1 1 calc R U . . .
C8 C 0.8681(3) 0.20781(18) 0.3449(2) 0.0408(9) Uani 1 1 d . . . . .
H8A H 0.9344 0.1950 0.3237 0.049 Uiso 1 1 calc R U . . .
C9 C 0.7626(3) 0.18965(16) 0.31046(18) 0.0325(7) Uani 1 1 d . . . . .
C10 C 0.7553(3) 0.15272(17) 0.24588(19) 0.0378(8) Uani 1 1 d . . . . .
H10A H 0.8223 0.1399 0.2257 0.045 Uiso 1 1 calc R U . . .
C11 C 0.6551(3) 0.13509(17) 0.2118(2) 0.0394(8) Uani 1 1 d . . . . .
H11A H 0.6521 0.1092 0.1696 0.047 Uiso 1 1 calc R U . . .
C12 C 0.5557(3) 0.15586(16) 0.24014(19) 0.0338(7) Uani 1 1 d . . . . .
H12A H 0.4856 0.1442 0.2156 0.041 Uiso 1 1 calc R U . . .
C13 C 0.5572(2) 0.19259(14) 0.30241(16) 0.0261(6) Uani 1 1 d . . . . .
C15 C 0.4471(2) 0.21603(14) 0.32207(16) 0.0254(6) Uani 1 1 d . . . . .
C16 C 0.3631(3) 0.17850(14) 0.34205(17) 0.0277(6) Uani 1 1 d . . . . .
H16A H 0.3760 0.1380 0.3441 0.033 Uiso 1 1 calc R U . . .
C17 C 0.2601(3) 0.20110(16) 0.35905(18) 0.0326(7) Uani 1 1 d . . . . .
Cl1 Cl 0.15845(7) 0.15377(5) 0.38595(6) 0.0486(2) Uani 1 1 d . . . . .
C18 C 0.2372(3) 0.25958(16) 0.35581(18) 0.0326(7) Uani 1 1 d . . . . .
H18A H 0.1668 0.2744 0.3678 0.039 Uiso 1 1 calc R U . . .
C19 C 0.3210(3) 0.29548(15) 0.33437(17) 0.0302(7) Uani 1 1 d . . . . .
Cl2 Cl 0.29626(8) 0.36970(4) 0.32959(5) 0.0419(2) Uani 1 1 d . . . . .
C20 C 0.4253(3) 0.27512(15) 0.31727(16) 0.0281(6) Uani 1 1 d . . . . .
H20A H 0.4809 0.3012 0.3025 0.034 Uiso 1 1 calc R U . . .
C21 C 0.9538(10) 0.5000 0.7137(6) 0.103(3) Uani 1 2 d S T P . .
H21A H 0.9552 0.4653 0.6807 0.124 Uiso 0.5 1 calc R U P A -1
H21B H 0.9552 0.5347 0.6807 0.124 Uiso 0.5 1 calc R U P A -1
Cl3 Cl 1.0678(2) 0.5000 0.78090(14) 0.0857(6) Uani 1 2 d S T P . .
Cl4 Cl 0.8292(3) 0.5000 0.7656(3) 0.1477(15) Uani 1 2 d S T P . .
C22 C 1.2391(8) 0.5000 0.5153(5) 0.097(3) Uani 1 2 d S T P . .
H22A H 1.1907 0.4654 0.5081 0.117 Uiso 0.5 1 calc R U P B -1
H22B H 1.1907 0.5346 0.5081 0.117 Uiso 0.5 1 calc R U P B -1
Cl5 Cl 1.3351(3) 0.5000 0.44601(12) 0.0965(9) Uani 1 2 d S T P . .
Cl6 Cl 1.30334(19) 0.5000 0.60864(11) 0.0736(5) Uani 1 2 d S T P . .
C23 C 0.5348(11) 0.5000 0.7784(8) 0.135(5) Uani 1 2 d S T P . .
H23A H 0.5357 0.5359 0.7488 0.202 Uiso 0.5 1 calc R U P C -1
H23B H 0.6038 0.4971 0.8124 0.202 Uiso 0.5 1 calc R U P C -1
H23C H 0.5298 0.4669 0.7433 0.202 Uiso 0.5 1 calc R U P C -1
C24 C 0.4403(9) 0.5000 0.8233(6) 0.092(3) Uani 1 2 d S T P . .
H24A H 0.3733 0.5000 0.7853 0.110 Uiso 1 2 calc R U P . .
C25 C 0.4271(5) 0.5533(3) 0.8729(4) 0.0880(19) Uani 1 1 d . . . . .
H25A H 0.4253 0.5881 0.8399 0.106 Uiso 1 1 calc R U . . .
H25B H 0.4932 0.5566 0.9105 0.106 Uiso 1 1 calc R U . . .
C26 C 0.3212(5) 0.5520(3) 0.9162(4) 0.0849(18) Uani 1 1 d . . . . .
H26A H 0.3211 0.5857 0.9510 0.102 Uiso 1 1 calc R U . . .
H26B H 0.2546 0.5550 0.8790 0.102 Uiso 1 1 calc R U . . .
C27 C 0.3140(8) 0.5000 0.9600(7) 0.089(3) Uani 1 2 d S T P . .
H27A H 0.3750 0.5000 1.0017 0.107 Uiso 1 2 calc R U P . .
H27B H 0.2420 0.5000 0.9842 0.107 Uiso 1 2 calc R U P . .
B1 B 1.0179(10) 0.6173(4) 0.4824(6) 0.048(3) Uani 0.5 1 d D . P D 1
F1 F 1.0576(5) 0.6621(3) 0.4407(4) 0.0602(16) Uani 0.5 1 d D . P D 1
F2 F 0.9233(7) 0.6366(4) 0.5164(6) 0.092(3) Uani 0.5 1 d D . P D 1
F3 F 0.9891(6) 0.5712(3) 0.4345(3) 0.0730(17) Uani 0.5 1 d D . P D 1
F4 F 1.0973(7) 0.5993(3) 0.5377(4) 0.082(2) Uani 0.5 1 d D . P D 1
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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
Ag Ag -0.8971 1.1015 '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
C1 Ag1 C1 35.1(3) . 2_656
C1 Ag1 N4 160.91(14) . 2_656
C1 Ag1 N4 126.39(15) 2_656 2_656
C1 Ag1 N4 126.39(15) . .
C1 Ag1 N4 160.91(14) 2_656 .
N4 Ag1 N4 72.46(13) 2_656 .
C3 N4 C5 124.1(3) . .
C3 N4 Ag1 117.37(19) . .
C5 N4 Ag1 117.9(2) . .
C1 C1 Ag1 72.47(13) 2_656 .
N4 C3 C2 125.6(3) . .
N4 C3 C3 116.22(17) . 2_656
C2 C3 C3 118.08(19) . 2_656
C9 C4 C5 116.5(3) . .
C9 C4 C13 118.0(3) . .
C5 C4 C13 125.4(3) . .
C6 C5 N4 118.9(3) . .
C6 C5 C4 121.5(3) . .
N4 C5 C4 118.9(3) . .
C5 C6 C7 120.6(3) . .
C8 C7 C6 119.7(3) . .
C7 C8 C9 121.7(3) . .
C10 C9 C8 120.9(3) . .
C10 C9 C4 119.4(3) . .
C8 C9 C4 119.7(3) . .
C11 C10 C9 121.8(3) . .
C10 C11 C12 119.0(3) . .
C13 C12 C11 121.9(3) . .
C12 C13 C4 119.6(3) . .
C12 C13 C15 116.7(3) . .
C4 C13 C15 123.5(3) . .
C20 C15 C16 119.4(3) . .
C20 C15 C13 120.5(3) . .
C16 C15 C13 120.1(3) . .
C17 C16 C15 119.3(3) . .
C18 C17 C16 122.4(3) . .
C18 C17 Cl1 119.2(2) . .
C16 C17 Cl1 118.4(3) . .
C19 C18 C17 117.0(3) . .
C18 C19 C20 122.8(3) . .
C18 C19 Cl2 118.8(2) . .
C20 C19 Cl2 118.4(3) . .
C19 C20 C15 119.2(3) . .
Cl3 C21 Cl4 107.4(6) . .
Cl5 C22 Cl6 112.6(6) . .
C23 C24 C25 115.8(6) . 6_565
C23 C24 C25 115.8(6) . .
C25 C24 C25 108.2(8) 6_565 .
C24 C25 C26 113.2(6) . .
C27 C26 C25 111.7(6) . .
C26 C27 C26 114.2(10) 6_565 .
B1 B1 F2 120(2) 2_756 2_756
B1 B1 F4 80.6(17) 2_756 .
F2 B1 F4 66.8(12) 2_756 .
B1 B1 F1 131.0(5) 2_756 .
F2 B1 F1 43.9(11) 2_756 .
F4 B1 F1 110.7(10) . .
B1 B1 F3 110.7(13) 2_756 .
F2 B1 F3 126.8(12) 2_756 .
F4 B1 F3 108.6(8) . .
F1 B1 F3 110.0(8) . .
B1 B1 F2 31.2(12) 2_756 .
F2 B1 F2 122.0(13) 2_756 .
F4 B1 F2 109.9(8) . .
F1 B1 F2 108.1(7) . .
F3 B1 F2 109.5(10) . .
B1 B1 F4 67.6(16) 2_756 2_756
F2 B1 F4 160.3(15) 2_756 2_756
F4 B1 F4 132.5(9) . 2_756
F1 B1 F4 116.7(8) . 2_756
F3 B1 F4 56.5(6) . 2_756
F2 B1 F4 53.7(7) . 2_756
B1 B1 F3 45.6(10) 2_756 2_756
F2 B1 F3 112.9(14) 2_756 2_756
F4 B1 F3 47.7(5) . 2_756
F1 B1 F3 155.6(9) . 2_756
F3 B1 F3 90.4(7) . 2_756
F2 B1 F3 75.9(5) . 2_756
F4 B1 F3 85.5(6) 2_756 2_756
F2 F1 B1 36.8(8) 2_756 .
B1 F2 F1 99.3(16) 2_756 2_756
B1 F2 F4 76.7(11) 2_756 2_756
F1 F2 F4 175.1(12) 2_756 2_756
B1 F2 B1 28.9(11) 2_756 .
F1 F2 B1 112.1(11) 2_756 .
F4 F2 B1 65.6(7) 2_756 .
F4 F3 B1 64.5(6) 2_756 .
F4 F3 B1 48.6(5) 2_756 2_756
B1 F3 B1 23.7(7) . 2_756
F2 F4 F3 118.8(7) 2_756 2_756
F2 F4 B1 36.5(5) 2_756 .
F3 F4 B1 83.7(7) 2_756 .
F2 F4 B1 60.7(5) 2_756 2_756
F3 F4 B1 58.9(6) 2_756 2_756
B1 F4 B1 31.8(8) . 2_756
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 C1 2.237(4) .
Ag1 C1 2.237(4) 2_656
Ag1 N4 2.241(3) 2_656
Ag1 N4 2.241(3) .
N4 C3 1.276(4) .
N4 C5 1.421(3) .
C1 C1 1.348(10) 2_656
C2 C3 1.500(5) .
C3 C3 1.519(6) 2_656
C4 C9 1.431(4) .
C4 C5 1.431(4) .
C4 C13 1.432(4) .
C5 C6 1.376(4) .
C6 C7 1.404(5) .
C7 C8 1.351(6) .
C8 C9 1.418(5) .
C9 C10 1.413(5) .
C10 C11 1.359(6) .
C11 C12 1.411(5) .
C12 C13 1.380(5) .
C13 C15 1.493(4) .
C15 C20 1.393(5) .
C15 C16 1.394(4) .
C16 C17 1.394(4) .
C17 C18 1.381(5) .
C17 Cl1 1.731(3) .
C18 C19 1.378(5) .
C19 C20 1.390(4) .
C19 Cl2 1.743(3) .
C21 Cl3 1.728(11) .
C21 Cl4 1.809(13) .
C22 Cl5 1.735(10) .
C22 Cl6 1.748(9) .
C23 C24 1.429(15) .
C24 C25 1.523(9) 6_565
C24 C25 1.523(9) .
C25 C26 1.529(8) .
C26 C27 1.432(9) .
C27 C26 1.432(9) 6_565
B1 B1 0.78(2) 2_756
B1 F2 0.834(12) 2_756
B1 F4 1.366(13) .
B1 F1 1.375(12) .
B1 F3 1.383(12) .
B1 F2 1.396(13) .
B1 F4 1.458(14) 2_756
B1 F3 1.810(12) 2_756
F1 F2 0.967(11) 2_756
F2 B1 0.834(12) 2_756
F2 F1 0.967(11) 2_756
F2 F4 1.290(12) 2_756
F3 F4 1.346(10) 2_756
F3 B1 1.810(12) 2_756
F4 F2 1.290(12) 2_756
F4 F3 1.346(10) 2_756
F4 B1 1.458(14) 2_756
