Novel Mn4-Co2 nanocluster@photosensitizers/SalenCo(iii) catalyze the copolymerization of carbon dioxide and propylene oxide
Yang, ZhiWei; Du, LongChao; RSC Advances 13 (2023) 13930–13939; doi:10.1039/D3RA01742G

data_7246763
_publ_section_title
;
 Novel Mn4-Co2 nanocluster@photosensitizers/SalenCo(iii) catalyze the
 copolymerization of carbon dioxide and propylene oxide
;
_journal_issue                   20
_journal_name_full               'RSC Advances'
_journal_page_first              13930
_journal_page_last               13939
_journal_paper_doi               10.1039/D3RA01742G
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C70 H110 Co2 Mn4 N4 O22, 1[C5N1H5], 1[]'
_chemical_formula_sum            'C70 H110 Co2 Mn4 N4 O22'
_chemical_formula_weight         1697.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1256(5)
_cell_length_b                   23.1528(7)
_cell_length_c                   28.0634(7)
_cell_measurement_reflns_used    18372
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.73
_cell_measurement_theta_min      3.82
_cell_volume                     9178.1(5)
_computing_cell_refinement
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 2.0, Darmstadt 2021
;
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details      '708 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 mm, 0.6 diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            22065
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         69.625
_diffrn_reflns_theta_min         3.818
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    7.624
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.801
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8249
_refine_ls_number_restraints     555
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+15.1499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6256
_reflns_number_total             8249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra01742g2.cif
_cod_data_source_block           2
_cod_database_code               7246763
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.273
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-C2 \\sim C12-C9
 with sigma of 0.02
 C12-C17 \\sim C12-C37
 with sigma of 0.02
 C33-C12 \\sim C9-C12 \\sim C2-C12 \\sim C37-C12 \\sim C17-C12 \\sim C35-C12
 with sigma of 0.02
 C12-C33 \\sim C12-C35
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C9 \\sim C12 \\sim C17 \\sim C33 \\sim C35 \\sim C37: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C15 \\sim C20 \\sim C29 \\sim C31: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C14 \\sim C5 \\sim C21 \\sim C38: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C9) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. 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
5. Others
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=1-FVAR(1)
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(1)
 Fixed X: C17(0.51014)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C11(H11), C13(H13), C19(H19), C22(H22), C24(H24), C26(H26), C27(H27),
 C32(H32), C34(H34)
6.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C15(H15A,
 H15B,H15C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C),
 C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              21453
_shelx_fab_checksum              89235
_platon_squeeze_special_details
;
A solvent mask was calculated and 172 electrons were 
found in a volume of 1328\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C5N1H5], 1[] per Asymmetric Unit 
which account for 168 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.172 mm'
_stoe_detector_pixelsize_y       '0.172 mm'
_stoe_detector_size_x            '8.4 cm'
_stoe_detector_size_y            '10.6 cm'
_stoe_evaluation_integration_a   6.0
_stoe_evaluation_integration_b   0.5
_stoe_evaluation_integration_ems 0.020
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 94.9
_stoe_evaluation_lana_dxs_max_order 3
_stoe_evaluation_lana_dys_max_order 3
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 139.4
_stoe_evaluation_lana_max_2theta_desired 139.4
_stoe_evaluation_lana_mean_redundancy 2.6
_stoe_evaluation_lana_number_refls_after_or 23473
_stoe_evaluation_lana_number_refls_outliers 6205
_stoe_evaluation_lana_number_refls_total 29678
_stoe_evaluation_lana_number_refls_unique 8981
_stoe_evaluation_lana_number_refls_written 23473
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group mmm
_stoe_evaluation_lana_table
;
2Theta          14.3   29.1   43.9   58.7   73.5   88.3  103.1  117.9  132.7
<Resolution>    4.99   2.95   2.05   1.57   1.27   1.11   0.99   0.90   0.85
N(total)         238   1081   2029   2620   5774   5540   5368   4637   2391
<Redundancy>     2.4    2.7    2.6    2.3    3.4    2.8    2.6    2.4    1.9
Complet. [%%]    82.8   97.1   98.5   95.9   97.3   99.7   99.5   96.5   78.5
<I/sigma>      272.1  161.5   96.8   46.4   16.8    9.8    7.6    5.1    4.5
R(int)         0.020  0.016  0.019  0.032  0.045  0.060  0.076  0.114  0.133
;
_stoe_measurement_identifier     2
_stoe_measurement_max_exposure_per_frame '20.0 s'
_stoe_measurement_mean_exposure_per_frame '16.8 s'
_stoe_measurement_min_exposure_per_frame '6.0 s'
_stoe_measurement_total_exposure_time '3.3 h'
_stoe_measurement_total_frame_number 708
_stoe_measurement_total_run_number 14
_stoe_measurement_tube_power     '30.0 W'