Isosmaragdyrin with an N<sub>3</sub>C<sub>2</sub> core: stabilization of Rh(i) and organo-Pt(ii) complexes.
Das, Mainak; Chitranshi, Sangya; Murugavel, M.; Adinarayana, B.; Suresh, Cherumuttathu H.; Srinivasan, A.; Chemical communications (Cambridge, England) 56 (2020) 3551–3554; doi:10.1039/d0cc00214c

data_7126037
_publ_section_title
;
 Isosmaragdyrin with an N<sub>3</sub>C<sub>2</sub> core: stabilization of
 Rh(i) and organo-Pt(ii) complexes.
;
_journal_issue                   24
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3551
_journal_page_last               3554
_journal_paper_doi               10.1039/d0cc00214c
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C52 H37 Cl F5 N3 Pt'
_chemical_formula_sum            'C52 H37 Cl F5 N3 Pt'
_chemical_formula_weight         1029.41
_chemical_name_systematic        Py-ism-Pt
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-01 deposited with the CCDC.	2020-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.548(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.6392(15)
_cell_length_b                   8.7956(4)
_cell_length_c                   37.084(2)
_cell_measurement_reflns_used    6781
_cell_measurement_temperature    299.2(4)
_cell_measurement_theta_max      72.9830
_cell_measurement_theta_min      3.7860
_cell_volume                     10300.2(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46b (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_environment      air
_diffrn_ambient_temperature      299.2(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -58.00 -10.00   0.50   20.00    --    0.00 139.00  21.00   96
  2  \w    -53.00  -6.00   0.50   20.00    --    0.00 130.00-152.00   94
  3  \w     40.00 121.00   0.50   20.00    --  102.08-130.00 135.00  162
  4  \w     80.00 105.00   0.50   20.00    --  102.08  77.00 -60.00   50
  5  \w     92.00 164.00   0.50   20.00    --  102.08 130.00-152.00  144
  6  \w     86.00 163.00   0.50   20.00    --  102.08 139.00  21.00  154
  7  \w     -1.00  65.00   0.50   20.00    --    0.00  37.00  30.00  132
  8  \w     -1.00  67.00   0.50   20.00    --    0.00  19.00-150.00  136
  9  \w     -1.00  65.00   0.50   20.00    --    0.00  37.00 -30.00  132
 10  \w     36.00 103.00   0.50   20.00    --  102.08 -30.00   0.00  134
 11  \w     36.00 103.00   0.50   20.00    --  102.08 -30.00  60.00  134
 12  \w     34.00 104.00   0.50   20.00    --  102.08 -15.00 -60.00  140
 13  \w     80.00 162.00   0.50   20.00    --  102.08  77.00 -60.00  164
 14  \w    136.00 162.00   0.50   20.00    --  102.08  77.00 -60.00   52
 15  \w     41.00 114.00   0.50   20.00    --  102.08 -61.00 120.00  146
 16  \w     43.00 108.00   0.50   20.00    --  102.08 -61.00 -90.00  130
 17  \w    104.00 130.00   0.50   20.00    --  102.08  15.00 -30.00   52
 18  \w    142.00 168.00   0.50   20.00    --  102.08  15.00 -30.00   52
 19  \w     47.00 105.00   0.50   20.00    --  102.08 -45.00 -90.00  116
 20  \w     91.00 146.00   0.50   20.00    --  102.08  61.00 120.00  110
 21  \w     40.00 105.00   0.50   20.00    --  102.08 -45.00   0.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0060739000
_diffrn_orient_matrix_UB_12      -0.0221794000
_diffrn_orient_matrix_UB_13      -0.0411962000
_diffrn_orient_matrix_UB_21      -0.0314692000
_diffrn_orient_matrix_UB_22      -0.1302459000
_diffrn_orient_matrix_UB_23      0.0057058000
_diffrn_orient_matrix_UB_31      -0.0368376000
_diffrn_orient_matrix_UB_32      0.1148133000
_diffrn_orient_matrix_UB_33      -0.0015023000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1227
_diffrn_reflns_av_unetI/netI     0.1117
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            39416
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         3.565
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.819
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic blackish blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             4593
_exptl_crystal_size_max          0.362
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.212
_refine_diff_density_max         4.556
_refine_diff_density_min         -1.811
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         9420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0907
_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/[\s^2^(Fo^2^)+(0.1740P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5832
_reflns_number_total             9420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00214c2.cif
_cod_data_source_block           as-py-ism-pt
_cod_depositor_comments
;
Adding full bibliography for 7126036--7126038.cif.

2025-03-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C400 H344 Cl F72 N80 Pt8'
_cod_original_formula_weight         9235.70
_cod_original_formula_moiety         '8(C52 H37 Cl F5 N3 Pt)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        10300.1(9)
_cod_database_code               7126037
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C400 H344 F72 N80 Pt8 Cl1 '
_diffrn_oxdiff_ac3_digest_frames
;
013085c9cd18619bfad3b8ad8e28dbbdba0002520a8
;
_diffrn_oxdiff_ac3_digest_hkl
;
01a1dff715459eb1e63657cee42954f106c416
;
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 N1(H1), C8(H8), C13(H13), C14(H14), C20(H20), C4(H4), C42(H42), C31(H31),
 C9(H9), C28(H28), C23(H23), C40(H40), C18(H18), C33(H33), C3(H3), C2(H2),
 C19(H19), C25(H25), C24(H24)
2.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C44(H44A,H44B,
 H44C), C36(H36A,H36B,H36C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              5980
_shelx_fab_checksum              4486
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.935
_oxdiff_exptl_absorpt_empirical_full_min 0.291