#------------------------------------------------------------------------------
#$Date: 2019-11-24 13:07:47 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237976 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/00/4350077.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_4350077
loop_
_publ_author_name
'Artem'ev, Alexander V.'
'Ryzhikov, Maxim R.'
'Berezin, Alexey S.'
'Kolesnikov, Ilya E.'
'Samsonenko, Denis G.'
'Bagryanskaya, Irina Yu.'
_publ_section_title
;
 Photoluminescence of Ag(i) complexes with a square-planar coordination
 geometry: the first observation
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2855
_journal_paper_doi               10.1039/C9QI00657E
_journal_volume                  6
_journal_year                    2019
_chemical_formula_sum            'C30 H24 Ag Cl N6 O6 P2'
_chemical_formula_weight         769.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-07-27 deposited with the CCDC.	2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.087(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6372(6)
_cell_length_b                   15.7157(9)
_cell_length_c                   12.0166(8)
_cell_measurement_reflns_used    5594
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      3.76
_cell_volume                     1567.26(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6168
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.850
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12110
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         29.617
_diffrn_reflns_theta_min         3.397
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       block
_exptl_crystal_F_000             776
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.843
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3743
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0863P)²+0.5148P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1344
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3219
_reflns_number_total             3743
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9qi00657e3.cif
_cod_data_source_block           D1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4350077
_shelx_shelxl_version_number     2018/3
_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   0.784
_shelx_estimated_absorpt_t_max   0.857
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.000000 0.500000 0.500000 0.04497(14) Uani 1 2 d S . P . .
O1 O 0.1290(3) 0.23024(12) 0.71327(19) 0.0586(6) Uani 1 1 d . . . . .
P1 P 0.09841(8) 0.30954(4) 0.64486(6) 0.03686(18) Uani 1 1 d . . . . .
C11 C 0.2247(3) 0.39652(15) 0.7175(2) 0.0362(5) Uani 1 1 d . . . . .
C12 C 0.3494(4) 0.38003(19) 0.8147(2) 0.0489(7) Uani 1 1 d . . . . .
H12 H 0.364454 0.325651 0.846422 0.059 Uiso 1 1 calc R U . . .
C13 C 0.4516(4) 0.4456(2) 0.8644(3) 0.0587(8) Uani 1 1 d . . . . .
H13 H 0.540112 0.435479 0.927572 0.070 Uiso 1 1 calc R U . . .
C14 C 0.4202(4) 0.5258(2) 0.8188(3) 0.0517(7) Uani 1 1 d . . . . .
H14 H 0.485516 0.571279 0.852458 0.062 Uiso 1 1 calc R U . . .
C15 C 0.2924(4) 0.53845(17) 0.7237(2) 0.0444(6) Uani 1 1 d . . . . .
H15 H 0.272016 0.593206 0.693946 0.053 Uiso 1 1 calc R U . . .
N1 N 0.1944(3) 0.47460(14) 0.67113(19) 0.0383(5) Uani 1 1 d . . . . .
C21 C 0.1401(3) 0.29950(15) 0.5062(2) 0.0367(5) Uani 1 1 d . . . . .
C22 C 0.2242(3) 0.22978(18) 0.4842(3) 0.0477(7) Uani 1 1 d . . . . .
H22 H 0.260594 0.187953 0.540103 0.057 Uiso 1 1 calc R U . . .
C23 C 0.2525(4) 0.2238(2) 0.3780(3) 0.0646(9) Uani 1 1 d . . . . .
H23 H 0.308451 0.177574 0.360261 0.078 Uiso 1 1 calc R U . . .
C24 C 0.1974(5) 0.2868(2) 0.2982(3) 0.0649(9) Uani 1 1 d . . . . .
H24 H 0.215636 0.283714 0.225567 0.078 Uiso 1 1 calc R U . . .
C25 C 0.1151(4) 0.3545(2) 0.3262(3) 0.0571(8) Uani 1 1 d . . . . .
H25 H 0.076791 0.396457 0.270885 0.069 Uiso 1 1 calc R U . . .
N2 N 0.0877(3) 0.36252(15) 0.4300(2) 0.0445(5) Uani 1 1 d . . . . .
C31 C -0.1094(3) 0.34588(18) 0.6064(2) 0.0401(6) Uani 1 1 d . . . . .
C32 C -0.1665(4) 0.40938(19) 0.6623(3) 0.0483(7) Uani 1 1 d . . . . .
H32 H -0.097620 0.440134 0.721913 0.058 Uiso 1 1 calc R U . . .
C33 C -0.3312(5) 0.4264(2) 0.6269(4) 0.0665(10) Uani 1 1 d . . . . .
H33 H -0.375006 0.469070 0.662489 0.080 Uiso 1 1 calc R U . . .
C34 C -0.4274(4) 0.3792(3) 0.5385(4) 0.0732(11) Uani 1 1 d . . . . .
H34 H -0.537582 0.389657 0.512765 0.088 Uiso 1 1 calc R U . . .
C35 C -0.3594(4) 0.3165(3) 0.4889(3) 0.0711(10) Uani 1 1 d . . . . .
H35 H -0.426151 0.284678 0.429468 0.085 Uiso 1 1 calc R U . . .
N3 N -0.2032(3) 0.2987(2) 0.5209(2) 0.0580(7) Uani 1 1 d . . . . .
Cl1 Cl 0.9860(9) 0.5066(4) 0.9963(6) 0.1009(11) Uani 0.5 1 d D U P A -1
O11 O 1.0175(13) 0.4336(4) 1.0640(7) 0.160(3) Uani 0.5 1 d D U P A -1
O12 O 0.8352(8) 0.4976(4) 0.9115(7) 0.127(2) Uani 0.5 1 d D U P A -1
O13 O 0.9763(11) 0.5785(4) 1.0643(6) 0.139(2) Uani 0.5 1 d D U P A -1
O14 O 1.1039(10) 0.5214(6) 0.9379(7) 0.119(2) Uani 0.5 1 d D U P A -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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
N1 Ag1 N1 180.0 . 3_566 yes
N1 Ag1 N2 86.40(8) . . yes
N1 Ag1 N2 86.40(8) 3_566 3_566 ?
N1 Ag1 N2 93.60(8) . 3_566 yes
N1 Ag1 N2 93.60(8) 3_566 . ?
N2 Ag1 N2 180.0 3_566 . yes
O1 P1 C11 112.17(12) . . ?
O1 P1 C21 112.91(13) . . ?
O1 P1 C31 114.75(14) . . ?
C11 P1 C31 107.77(12) . . ?
C21 P1 C11 105.22(12) . . ?
C21 P1 C31 103.19(12) . . ?
C12 C11 P1 119.4(2) . . ?
N1 C11 P1 117.81(18) . . ?
N1 C11 C12 122.8(2) . . ?
C11 C12 H12 120.6 . . ?
C11 C12 C13 118.9(3) . . ?
C13 C12 H12 120.6 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.8(3) . . ?
C14 C13 H13 120.6 . . ?
C13 C14 H14 120.3 . . ?
C15 C14 C13 119.4(3) . . ?
C15 C14 H14 120.3 . . ?
C14 C15 H15 118.7 . . ?
N1 C15 C14 122.7(3) . . ?
N1 C15 H15 118.7 . . ?
C11 N1 Ag1 122.65(17) . . ?
C11 N1 C15 117.3(2) . . ?
C15 N1 Ag1 119.78(19) . . ?
C22 C21 P1 119.8(2) . . ?
N2 C21 P1 116.78(19) . . ?
N2 C21 C22 123.5(3) . . ?
C21 C22 H22 120.9 . . ?
C23 C22 C21 118.2(3) . . ?
C23 C22 H22 120.9 . . ?
C22 C23 H23 120.4 . . ?
C22 C23 C24 119.2(3) . . ?
C24 C23 H23 120.4 . . ?
C23 C24 H24 120.3 . . ?
C23 C24 C25 119.4(3) . . ?
C25 C24 H24 120.3 . . ?
C24 C25 H25 118.7 . . ?
N2 C25 C24 122.6(3) . . ?
N2 C25 H25 118.7 . . ?
C21 N2 Ag1 118.86(17) . . ?
C25 N2 Ag1 122.8(2) . . ?
C25 N2 C21 117.0(3) . . ?
C32 C31 P1 124.7(2) . . ?
N3 C31 P1 111.4(2) . . ?
N3 C31 C32 123.7(3) . . ?
C31 C32 H32 121.1 . . ?
C31 C32 C33 117.8(3) . . ?
C33 C32 H32 121.1 . . ?
C32 C33 H33 120.6 . . ?
C34 C33 C32 118.7(3) . . ?
C34 C33 H33 120.6 . . ?
C33 C34 H34 120.4 . . ?
C35 C34 C33 119.1(3) . . ?
C35 C34 H34 120.4 . . ?
C34 C35 H35 118.2 . . ?
N3 C35 C34 123.5(4) . . ?
N3 C35 H35 118.2 . . ?
C35 N3 C31 117.1(3) . . ?
O11 Cl1 O12 109.2(4) . . ?
O11 Cl1 O13 110.8(4) . . ?
O11 Cl1 O14 112.1(4) . . ?
O13 Cl1 O12 107.8(4) . . ?
O14 Cl1 O12 107.8(4) . . ?
O14 Cl1 O13 108.9(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 N1 2.301(2) . yes
Ag1 N1 2.301(2) 3_566 ?
Ag1 N2 2.511(2) . yes
Ag1 N2 2.511(2) 3_566 ?
O1 P1 1.4759(19) . ?
P1 C11 1.815(3) . ?
P1 C21 1.806(3) . ?
P1 C31 1.817(3) . ?
C11 C12 1.376(4) . ?
C11 N1 1.343(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.380(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.372(5) . ?
C14 H14 0.9300 . ?
C14 C15 1.366(4) . ?
C15 H15 0.9300 . ?
C15 N1 1.352(4) . ?
C21 C22 1.380(4) . ?
C21 N2 1.340(3) . ?
C22 H22 0.9300 . ?
C22 C23 1.368(5) . ?
C23 H23 0.9300 . ?
C23 C24 1.368(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.373(5) . ?
C25 H25 0.9300 . ?
C25 N2 1.337(4) . ?
C31 C32 1.369(4) . ?
C31 N3 1.342(4) . ?
C32 H32 0.9300 . ?
C32 C33 1.393(5) . ?
C33 H33 0.9300 . ?
C33 C34 1.371(6) . ?
C34 H34 0.9300 . ?
C34 C35 1.366(6) . ?
C35 H35 0.9300 . ?
C35 N3 1.326(5) . ?
Cl1 O11 1.389(4) . ?
Cl1 O12 1.422(5) . ?
Cl1 O13 1.410(5) . ?
Cl1 O14 1.407(5) . ?
