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_7126038
_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         'C54 H38 F5 N3 O2 Rh'
_chemical_formula_sum            'C54 H39 F5 N3 O2 Rh'
_chemical_formula_weight         959.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-01-03
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.7471(2)
_cell_length_b                   24.2024(4)
_cell_length_c                   35.7587(13)
_cell_measurement_reflns_used    18253
_cell_measurement_temperature    296.87(10)
_cell_measurement_theta_max      75.9730
_cell_measurement_theta_min      3.8350
_cell_volume                     11031.9(5)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.87(10)
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.926
_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    -44.00   6.00   0.50    1.00    --    0.00 115.00-137.00  100
  2  \w     36.00 113.00   0.50    4.00    --  102.08-115.00 132.00  154
  3  \w     99.00 168.00   0.50    4.00    --  102.08 115.00-137.00  138
  4  \w     64.00 157.00   0.50    4.00    --  102.08 169.00   6.00  186
  5  \w    -67.00   1.00   0.50    1.00    --    0.00 -19.00 150.00  136
  6  \w    -65.00   1.00   0.50    1.00    --    0.00 -37.00  60.00  132
  7  \w     34.00 104.00   0.50    4.00    --  102.08 -15.00 120.00  140
  8  \w     39.00 105.00   0.50    4.00    --  102.08 -45.00 150.00  132
  9  \w     40.00 114.00   0.50    4.00    --  102.08 -61.00  60.00  148
 10  \w     39.00 105.00   0.50    4.00    --  102.08 -45.00  60.00  132
 11  \w    100.00 165.00   0.50    4.00    --  102.08  45.00  30.00  130
 12  \w     40.00 114.00   0.50    4.00    --  102.08 -61.00 150.00  148
 13  \w     36.00 103.00   0.50    4.00    --  102.08 -30.00  60.00  134
 14  \w    101.00 169.00   0.50    4.00    --  102.08  30.00 -30.00  136
 15  \w     39.00 105.00   0.50    4.00    --  102.08 -45.00 -90.00  132
 16  \w     49.00 140.00   0.50    4.00    --  102.08-169.00 -11.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0730
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            22736
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         84.760
_diffrn_reflns_theta_min         3.856
_exptl_absorpt_coefficient_mu    2.958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46997
_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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             3920
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.885
_refine_diff_density_min         -2.488
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11555
_refine_ls_number_restraints     582
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.1014
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2736
_refine_ls_wR_factor_ref         0.2901
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.924
_reflns_number_gt                9035
_reflns_number_total             11555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00214c2.cif
_cod_data_source_block           as-py-ism-rh
_cod_depositor_comments
'Adding full bibliography for 7126036--7126038.cif.'
_cod_database_code               7126038
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.718
_shelx_estimated_absorpt_t_min   0.562
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.49(2)
 0.51(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C48-C47 \\sim C52-C51 \\sim C50-C49
 with sigma of 0.02
4. Rigid bond restraints
 C28, C17, C18, C19, C20, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, O2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 C36(H36A,H36B,H36C)
6.b Ternary CH refined with riding coordinates:
 C39(H39)
6.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C27(H27), C4(H4), C3(H3), C28(H28), C25(H25), C18(H18),
 C33(H33), C20(H20), C23(H23), C24(H24), C19(H19), C2(H2), C9(H9), C31(H31),
 C42(H42), C8(H8), C40(H40)
6.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C46(H46A,H46B,H46C), C35(H35A,H35B,H35C), C44(H44A,H44B,
 H44C), C45(H45A,H45B,H45C)
;
_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
;