#------------------------------------------------------------------------------
#$Date: 2024-04-24 03:02:58 +0200 (Wed 24 de Apr de 2024) $
#$Revision: 291344 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/85/7248515.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_7248515
loop_
_publ_author_name
'Thakur, Vasudha'
'Thomas, Jisha Mary'
'Adnan, Mohammad'
'Sivasankar, Chinnappan'
'Vijaya Prakash, G.'
'Thirupathi, Natesan'
_publ_section_title
;
 Syntheses, structural, photophysical and theoretical studies of
 heteroleptic cycloplatinated guanidinate(1−) complexes bearing
 acetylacetonate and picolinate ancillary ligands
;
_journal_issue                   19
_journal_name_full               'RSC Advances'
_journal_page_first              13291
_journal_page_last               13305
_journal_paper_doi               10.1039/D4RA00828F
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C24 H20 Br3 N3 O2 Pt'
_chemical_formula_sum            'C24 H20 Br3 N3 O2 Pt'
_chemical_formula_weight         817.25
_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
_audit_creation_date             2018-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-28 deposited with the CCDC.	2024-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.627(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8997(3)
_cell_length_b                   13.5956(4)
_cell_length_c                   18.9893(5)
_cell_measurement_reflns_used    4596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.1000
_cell_measurement_theta_min      3.5650
_cell_volume                     2519.82(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9853
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1461
_diffrn_reflns_av_unetI/netI     0.1202
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.569
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    10.352
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.031
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.0690
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.2107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2697
_reflns_number_total             5136
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra00828f3.cif
_cod_data_source_block           Complex-17
_cod_database_code               7248515
_shelx_shelxl_version_number     2017/1
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), N2(H2), C16(H16), C17(H17), C18(H18), C3(H3A), C4(H4), C5(H5), C6(H6),
  C9(H9), C10(H10), C11(H11), C12(H12), C22(H22)
2.b Fitted hexagon refined as free rotating group:
 C15(C16,C17,C18,C19,C14), C2(C3,C4,C5,C6,C7), C8(C9,C10,C11,C12,C13)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C24(H24A,H24B,H24C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
Pt1 Pt 0.49553(6) 0.46475(4) 0.72718(3) 0.0542(3) Uani 1 1 d . . . . .
Br2 Br -0.00034(17) 0.27458(14) 0.46527(10) 0.0793(6) Uani 1 1 d . . . . .
Br3 Br 0.65084(19) 0.36519(15) 0.45136(9) 0.0779(6) Uani 1 1 d . . . . .
Br1 Br 0.4463(3) 0.16756(16) 0.73459(12) 0.1056(7) Uani 1 1 d . . . . .
O1 O 0.6202(10) 0.5599(7) 0.7896(5) 0.059(3) Uani 1 1 d . . . . .
O2 O 0.3695(10) 0.4542(8) 0.8049(5) 0.064(3) Uani 1 1 d . . . . .
N1 N 0.3692(12) 0.3697(8) 0.6679(6) 0.053(3) Uani 1 1 d . . . . .
N3 N 0.4695(12) 0.3720(9) 0.5652(6) 0.059(3) Uani 1 1 d . . . . .
H3 H 0.454083 0.358686 0.520325 0.070 Uiso 1 1 calc R . . . .
N2 N 0.2752(13) 0.2780(10) 0.5660(7) 0.071(4) Uani 1 1 d . . . . .
H2 H 0.202079 0.271211 0.584412 0.085 Uiso 1 1 calc R . . . .
C15 C 0.6208(10) 0.4719(7) 0.6542(4) 0.060(4) Uani 1 1 d . . . . .
C16 C 0.7403(12) 0.5267(8) 0.6713(4) 0.074(5) Uani 1 1 d G . . . .
H16 H 0.759585 0.559035 0.714976 0.089 Uiso 1 1 calc R . . . .
C17 C 0.8311(10) 0.5332(8) 0.6230(6) 0.088(6) Uani 1 1 d G . . . .
H17 H 0.911134 0.569893 0.634388 0.106 Uiso 1 1 calc R . . . .
C18 C 0.8024(10) 0.4850(8) 0.5577(5) 0.073(5) Uani 1 1 d G . . . .
H18 H 0.863148 0.489306 0.525376 0.088 Uiso 1 1 calc R . . . .
C19 C 0.6828(11) 0.4302(7) 0.5406(4) 0.055(4) Uani 1 1 d G . . . .
C14 C 0.5920(9) 0.4237(7) 0.5889(5) 0.060(4) Uani 1 1 d G . . . .
C2 C 0.2643(10) 0.3263(7) 0.7009(5) 0.054(4) Uani 1 1 d . . . . .
C3 C 0.1423(12) 0.3772(7) 0.7000(6) 0.079(5) Uani 1 1 d G . . . .
H3A H 0.128090 0.436929 0.676046 0.095 Uiso 1 1 calc R . . . .
C4 C 0.0415(10) 0.3389(10) 0.7351(6) 0.085(5) Uani 1 1 d G . . . .
H4 H -0.040160 0.372940 0.734513 0.102 Uiso 1 1 calc R . . . .
C5 C 0.0627(13) 0.2496(10) 0.7709(5) 0.088(6) Uani 1 1 d G . . . .
H5 H -0.004759 0.223979 0.794353 0.106 Uiso 1 1 calc R . . . .
C6 C 0.1847(15) 0.1987(7) 0.7717(5) 0.085(6) Uani 1 1 d G . . . .
H6 H 0.198894 0.139006 0.795727 0.102 Uiso 1 1 calc R . . . .
C7 C 0.2855(11) 0.2371(7) 0.7367(5) 0.067(4) Uani 1 1 d G . . . .
C1 C 0.3760(18) 0.3414(10) 0.6006(8) 0.058(4) Uani 1 1 d . . . . .
C8 C 0.2831(11) 0.2259(8) 0.5052(4) 0.059(4) Uani 1 1 d . . . . .
C9 C 0.4038(9) 0.1801(8) 0.4950(6) 0.077(5) Uani 1 1 d G . . . .
H9 H 0.481488 0.184373 0.530005 0.093 Uiso 1 1 calc R . . . .
C10 C 0.4084(12) 0.1278(9) 0.4326(8) 0.116(8) Uani 1 1 d G . . . .
H10 H 0.489210 0.097133 0.425753 0.139 Uiso 1 1 calc R . . . .
C11 C 0.2923(16) 0.1214(9) 0.3803(6) 0.109(8) Uani 1 1 d G . . . .
H11 H 0.295417 0.086409 0.338530 0.131 Uiso 1 1 calc R . . . .
C12 C 0.1716(12) 0.1672(9) 0.3905(5) 0.086(6) Uani 1 1 d G . . . .
H12 H 0.093901 0.162926 0.355559 0.103 Uiso 1 1 calc R . . . .
C13 C 0.1670(9) 0.2195(8) 0.4530(5) 0.063(4) Uani 1 1 d G . . . .
C21 C 0.6005(18) 0.5867(14) 0.8509(8) 0.075(5) Uani 1 1 d . . . . .
C23 C 0.3877(19) 0.5051(16) 0.8635(9) 0.079(5) Uani 1 1 d . . . . .
C22 C 0.4948(19) 0.5647(13) 0.8888(9) 0.077(5) Uani 1 1 d . . . . .
H22 H 0.498074 0.592481 0.933803 0.093 Uiso 1 1 calc R . . . .
C20 C 0.709(2) 0.6626(15) 0.8848(9) 0.101(7) Uani 1 1 d . . . . .
H20A H 0.795736 0.630177 0.898770 0.152 Uiso 1 1 calc GR . . . .
H20B H 0.680774 0.691609 0.926022 0.152 Uiso 1 1 calc GR . . . .
H20C H 0.718648 0.713121 0.850589 0.152 Uiso 1 1 calc GR . . . .
C24 C 0.2831(18) 0.4806(15) 0.9105(9) 0.087(6) Uani 1 1 d . . . . .
H24A H 0.197476 0.511640 0.891693 0.131 Uiso 1 1 calc GR . . . .
H24B H 0.314812 0.504067 0.958037 0.131 Uiso 1 1 calc GR . . . .
H24C H 0.270498 0.410659 0.911462 0.131 Uiso 1 1 calc GR . . . .
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 '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
O1 Pt1 O2 90.5(4) . . ?
N1 Pt1 O1 178.3(4) . . ?
N1 Pt1 O2 87.9(4) . . ?
N1 Pt1 C15 92.5(4) . . ?
C15 Pt1 O1 89.2(4) . . ?
C15 Pt1 O2 178.2(4) . . ?
C21 O1 Pt1 123.3(11) . . ?
C23 O2 Pt1 123.7(12) . . ?
C2 N1 Pt1 116.8(8) . . ?
C1 N1 Pt1 126.2(11) . . ?
C1 N1 C2 117.0(12) . . ?
C14 N3 H3 114.9 . . ?
C1 N3 H3 114.9 . . ?
C1 N3 C14 130.1(12) . . ?
C1 N2 H2 117.3 . . ?
C8 N2 H2 117.3 . . ?
C8 N2 C1 125.4(13) . . ?
C16 C15 Pt1 117.7(6) . . ?
C16 C15 C14 120.0 . . ?
C14 C15 Pt1 122.3(6) . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C18 C17 H17 120.0 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 Br3 117.9(6) . . ?
C18 C19 C14 120.0 . . ?
C14 C19 Br3 122.1(6) . . ?
C15 C14 N3 123.9(8) . . ?
C19 C14 N3 116.0(8) . . ?
C19 C14 C15 120.0 . . ?
C3 C2 N1 119.0(9) . . ?
C3 C2 C7 120.0 . . ?
C7 C2 N1 120.9(9) . . ?
C2 C3 H3A 120.0 . . ?
C2 C3 C4 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C2 C7 Br1 119.6(7) . . ?
C6 C7 Br1 120.4(7) . . ?
C6 C7 C2 120.0 . . ?
N1 C1 N2 118.6(16) . . ?
N3 C1 N1 123.5(15) . . ?
N3 C1 N2 117.9(13) . . ?
N2 C8 C9 121.4(9) . . ?
N2 C8 C13 118.6(9) . . ?
C9 C8 C13 120.0 . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C10 C11 C12 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C8 C13 Br2 122.0(6) . . ?
C12 C13 Br2 117.9(6) . . ?
C12 C13 C8 120.0 . . ?
O1 C21 C22 131.0(16) . . ?
O1 C21 C20 111.8(17) . . ?
C22 C21 C20 117.1(14) . . ?
O2 C23 C22 127.7(17) . . ?
O2 C23 C24 112.2(17) . . ?
C22 C23 C24 119.6(16) . . ?
C21 C22 H22 118.2 . . ?
C23 C22 C21 123.6(16) . . ?
C23 C22 H22 118.2 . . ?
C21 C20 H20A 109.5 . . ?
C21 C20 H20B 109.5 . . ?
C21 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
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
Pt1 O1 2.027(9) . ?
Pt1 O2 2.091(10) . ?
Pt1 N1 2.008(11) . ?
Pt1 C15 2.010(8) . ?
Br2 C13 1.868(9) . ?
Br3 C19 1.891(7) . ?
Br1 C7 1.857(10) . ?
O1 C21 1.265(16) . ?
O2 C23 1.296(19) . ?
N1 C2 1.427(13) . ?
N1 C1 1.346(17) . ?
N3 H3 0.8600 . ?
N3 C14 1.409(13) . ?
N3 C1 1.300(19) . ?
N2 H2 0.8600 . ?
N2 C1 1.396(19) . ?
N2 C8 1.367(14) . ?
C15 C16 1.3900 . ?
C15 C14 1.3900 . ?
C16 H16 0.9300 . ?
C16 C17 1.3900 . ?
C17 H17 0.9300 . ?
C17 C18 1.3900 . ?
C18 H18 0.9300 . ?
C18 C19 1.3900 . ?
C19 C14 1.3900 . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 H3A 0.9300 . ?
C3 C4 1.3900 . ?
C4 H4 0.9300 . ?
C4 C5 1.3900 . ?
C5 H5 0.9300 . ?
C5 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C7 1.3900 . ?
C8 C9 1.3900 . ?
C8 C13 1.3900 . ?
C9 H9 0.9300 . ?
C9 C10 1.3900 . ?
C10 H10 0.9300 . ?
C10 C11 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 H12 0.9300 . ?
C12 C13 1.3900 . ?
C21 C22 1.40(2) . ?
C21 C20 1.55(2) . ?
C23 C22 1.36(2) . ?
C23 C24 1.51(2) . ?
C22 H22 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
