Designing a Cr-catalyst bearing redox non-innocent phenalenyl-based ligand towards hydrosilylative CO<sub>2</sub> functionalization.
Chakraborty, Soumi; Das, Arpan; Ahmed, Jasimuddin; Barman, Sayani; Mandal, Swadhin K.; Chemical communications (Cambridge, England) 56 (2020) 13788–13791; doi:10.1039/d0cc05348a

data_7127349
_publ_section_title
;
 Designing a Cr-catalyst bearing redox non-innocent phenalenyl-based
 ligand towards hydrosilylative CO<sub>2</sub> functionalization.
;
_journal_issue                   89
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13788
_journal_page_last               13791
_journal_paper_doi               10.1039/d0cc05348a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C38 H26 Cr N4 O2, Cl, 2(C H4 O), H2 O'
_chemical_formula_sum            'C40 H36 Cl Cr N4 O5'
_chemical_formula_weight         740.17
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-08 deposited with the CCDC.	2020-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                83.383(5)
_cell_angle_beta                 76.246(6)
_cell_angle_gamma                89.429(5)
_cell_formula_units_Z            4
_cell_length_a                   9.8879(7)
_cell_length_b                   16.9397(10)
_cell_length_c                   20.5976(14)
_cell_measurement_reflns_used    5420
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      25.0760
_cell_measurement_theta_min      2.1080
_cell_volume                     3328.3(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.754
_diffrn_measured_fraction_theta_max 0.753
_diffrn_measurement_details
;
  1 omega  -33.00   66.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1679  -57.0000  -60.0000 99

  2 omega  -44.00  -18.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1679  -57.0000 -180.0000 26

  3 omega   18.00   63.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1679  -57.0000 -180.0000 45

  4 omega  -11.00   64.00   1.0000  125.0000
omega____ theta____ kappa____ phi______ frames
    -       27.1679   57.0000  150.0000 75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0227104000
_diffrn_orient_matrix_UB_12      -0.0228021000
_diffrn_orient_matrix_UB_13      0.0318418000
_diffrn_orient_matrix_UB_21      -0.0580312000
_diffrn_orient_matrix_UB_22      -0.0142418000
_diffrn_orient_matrix_UB_23      -0.0101880000
_diffrn_orient_matrix_UB_31      0.0396564000
_diffrn_orient_matrix_UB_32      -0.0324768000
_diffrn_orient_matrix_UB_33      -0.0125088000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.754
_diffrn_reflns_Laue_measured_fraction_max 0.753
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10387
_diffrn_reflns_point_group_measured_fraction_full 0.754
_diffrn_reflns_point_group_measured_fraction_max 0.753
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.022
_diffrn_reflns_theta_min         1.674
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       plate
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.839
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         8861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.1025
_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^)+(0.0925P)^2^+32.1170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2616
_refine_ls_wR_factor_ref         0.2673
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7820
_reflns_number_total             8861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05348a2.cif
_cod_data_source_block           cr_nno
_cod_depositor_comments
;
Adding full bibliography for 7127348--7127349.cif.

2024-11-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety
'2(C38 H26 Cr N4 O2), 2(Cl), 4(C H4 O), 2(H2 O)'
_cod_original_formula_sum        'C80 H72 Cl2 Cr2 N8 O10'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1480.35
_cod_database_code               7127349
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N O Cu Cl'
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.890
_reflns_odcompleteness_completeness 70.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.63
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H5A of O5, H7A of O7, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H8 of O8, H10A of O10, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C21) = Uanis(C22)
Uanis(C36) = Uanis(C45) = Uanis(C37)
3.a Free rotating group:
 O6(H6A,H6B), O9(H9A,H9B)
3.b Rotating group:
 O7(H7A)
3.c Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C52(H52A,H52B), C46(H46A,H46B), C71(H71A,H71B)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C28(H28),
  C29(H29), C54(H54), C55(H55), C56(H56), C57(H57), C34(H34), C35(H35),
 C37(H37), C38(H38), C39(H39), C41(H41), C42(H42), C48(H48), C49(H49), C50(H50),
  C51(H51), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C66(H66),
 C67(H67), C73(H73), C74(H74), C75(H75), C76(H76)
3.e Idealised Me refined as rotating group:
 C80(H80B,H80C,H80A), C79(H79A,H79B,H79C), C78(H78A,H78B,H78C), C77(H77A,H77B,
 H77C)
3.f Idealised tetrahedral OH refined as rotating group:
 O8(H8), O10(H10A)
;
_shelx_res_checksum              86104
_olex2_submission_special_instructions 'No special instructions were received'