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_7126036
_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 H38 F5 N3'
_chemical_formula_sum            'C52 H38 F5 N3'
_chemical_formula_weight         799.85
_chemical_name_systematic        'core-modified isosmaragdyrin'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-10-01 deposited with the CCDC.	2020-02-17 downloaded from the CCDC.
;
_cell_angle_alpha                111.513(4)
_cell_angle_beta                 112.548(4)
_cell_angle_gamma                93.946(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1765(4)
_cell_length_b                   13.0482(6)
_cell_length_c                   15.2310(5)
_cell_measurement_reflns_used    5958
_cell_measurement_temperature    100
_cell_measurement_theta_max      75.1640
_cell_measurement_theta_min      3.7520
_cell_volume                     2016.53(17)
_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_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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    -65.00   1.00   0.50   14.00    --    0.00 -35.00 -57.00  132
  2  \w     -1.00  66.00   0.50   14.00    --    0.00  35.00  99.00  134
  3  \w     37.00 103.00   0.50   14.00    --  102.08 -35.00 -57.00  132
  4  \w    101.00 168.00   0.50   14.00    --  102.08  35.00  99.00  134
  5  \w    -22.00  62.00   0.50   14.00    --    0.00  77.00   0.00  168
  6  \w    -10.00  61.00   0.50   14.00    --    0.00  57.00-150.00  142
  7  \w    -10.00  61.00   0.50   14.00    --    0.00  57.00-180.00  142
  8  \w    -65.00   1.00   0.50   14.00    --    0.00 -37.00 -90.00  132
  9  \w    100.00 165.00   0.50   14.00    --  102.08  45.00  60.00  130
 10  \w     40.00 124.00   0.50   14.00    --  102.08 -77.00 150.00  168
 11  \w     39.00 118.00   0.50   14.00    --  102.08-125.00   0.00  158
 12  \w     39.00 105.00   0.50   14.00    --  102.08 -45.00-120.00  132
 13  \w    101.00 169.00   0.50   14.00    --  102.08  30.00 150.00  136
 14  \w     40.00 124.00   0.50   14.00    --  102.08 -77.00 -60.00  168
 15  \w     39.00 118.00   0.50   14.00    --  102.08-125.00 -60.00  158
 16  \w     39.00 105.00   0.50   14.00    --  102.08 -45.00  90.00  132
 17  \w     34.00 109.00   0.50   14.00    --  102.08 -94.00-180.00  150
 18  \w     36.00 103.00   0.50   14.00    --  102.08 -30.00-180.00  134
 19  \w     34.00 109.00   0.50   14.00    --  102.08 -94.00  60.00  150
 20  \w     39.00 118.00   0.50   14.00    --  102.08-125.00-180.00  158
 21  \w     36.00 103.00   0.50   14.00    --  102.08 -30.00 120.00  134
 22  \w    100.00 165.00   0.50   14.00    --  102.08  45.00 -60.00  130
 23  \w     34.00 104.00   0.50   14.00    --  102.08 -15.00 -60.00  140
 24  \w     40.00 114.00   0.50   14.00    --  102.08 -61.00 150.00  148
 25  \w     39.00 118.00   0.50   14.00    --  102.08-125.00  60.00  158
 26  \w     34.00 104.00   0.50   14.00    --  102.08 -15.00   0.00  140
 27  \w     40.00 114.00   0.50   14.00    --  102.08 -61.00  30.00  148
 28  \w     34.00 109.00   0.50   14.00    --  102.08 -94.00 120.00  150
 29  \w    100.00 165.00   0.50   14.00    --  102.08  45.00 -30.00  130
 30  \w     94.00 166.00   0.50   14.00    --  102.08 125.00 -30.00  144
 31  \w    -22.00  62.00   0.50   14.00    --    0.00  77.00  90.00  168
 32  \w     -1.00  67.00   0.50   14.00    --    0.00  19.00 -60.00  136
;
_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      0.0420688000
_diffrn_orient_matrix_UB_12      0.1305918000
_diffrn_orient_matrix_UB_13      0.0509601000
_diffrn_orient_matrix_UB_21      0.1321337000
_diffrn_orient_matrix_UB_22      -0.0079585000
_diffrn_orient_matrix_UB_23      0.0187504000
_diffrn_orient_matrix_UB_31      -0.0268922000
_diffrn_orient_matrix_UB_32      -0.0023556000
_diffrn_orient_matrix_UB_33      -0.1082364000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.2074
_diffrn_reflns_av_unetI/netI     0.1433
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28909
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.224
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36762
_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 yellowish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.729
_exptl_crystal_size_mid          0.452
_exptl_crystal_size_min          0.192
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0804
_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/[\s^2^(Fo^2^)+(0.1447P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2193
_refine_ls_wR_factor_ref         0.2602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4130
_reflns_number_total             7384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00214c2.cif
_cod_data_source_block           as_md_py_is
_cod_depositor_comments
'Adding full bibliography for 7126036--7126038.cif.'
_cod_original_cell_volume        2016.53(15)
_cod_database_code               7126036
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N F'
_diffrn_oxdiff_ac3_digest_frames
;
01c7f9688c89d0431144712f73be883c8504616840e
;
_diffrn_oxdiff_ac3_digest_hkl
;
0132b94bd5e7e4ce479a15b06786687185d499
;
_reflns_odcompleteness_completeness 100.00
_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. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(N2) = Uanis(N3)
3. Rigid body (RIGU) restrains
 N1, N2, N3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C28(H28), C13(H13), C27(H27), C8(H8), C19(H19), C3(H3), C20(H20),
 C25(H25), C2(H2), C9(H9), C4(H4), C18(H18), C23(H23), C33(H33), C42(H42),
 C40(H40), C24(H24), C31(H31), N1(H1)
4.b Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C37(H37A,H37B,H37C), C35(H35A,H35B,H35C), C44(H44A,H44B,
 H44C), C36(H36A,H36B,H36C), C45(H45A,H45B,H45C)
;
_olex2_submission_original_sample_id ISM
_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 6.673
_oxdiff_exptl_absorpt_empirical_full_min 0.263