A highly stable MnII phosphonate as highly efficient catalyst for CO2 fixation under ambient conditions
Yang, Yang; Gao, Chaoying; Tian, Hong-Rui; Ai, Jing; Min, Xue; Sun, Zhong-Ming; Chemical Communications  (2018) –; doi:10.1039/C7CC09867G

data_7121141
_publ_section_title
;
 A highly stable MnII phosphonate as highly efficient catalyst for CO2
 fixation under ambient conditions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC09867G
_journal_year                    2018
_chemical_formula_moiety         '0.03(C90 H116.93 Mn18 N18 O90 P18)'
_chemical_formula_sum            'C2.5 H4.25 Mn0.5 N0.5 O2.75 P0.5'
_chemical_formula_weight         128.24
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-06-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-29 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            36
_cell_length_a                   28.9848(19)
_cell_length_b                   28.9848(19)
_cell_length_c                   5.5266(7)
_cell_measurement_reflns_used    1738
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.43
_cell_volume                     4021.0(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            8289
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.041
_diffrn_reflns_theta_min         2.434
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1155 before and 0.0679 after correction.
The Ratio of minimum to maximum transmission is 0.8358.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_description       block
_exptl_crystal_F_000             2330
_refine_diff_density_max         2.354
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0802P)^2^+52.8081P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1628
_refine_ls_wR_factor_ref         0.1686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1475
_reflns_number_total             1763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09867g2.cif
_cod_data_source_block           mn
_cod_original_cell_volume        4021.0(7)
_cod_original_formula_sum        'C2.50 H4.25 Mn0.50 N0.50 O2.75 P0.50'
_cod_database_code               7121141
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C2')
Uanis(C3) = Uanis(C3')
Uanis(C4) = Uanis(C4')
Uanis(C5) = Uanis(C5')
3. Others
 Sof(C2')=Sof(H2')=Sof(C3')=Sof(H3')=Sof(C4')=Sof(H4')=Sof(C5')=Sof(H5')=1-
 FVAR(1)
 Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=FVAR(1)
4.a Rotating group:
 O1W(H1WA,H1WB)
4.b Ternary CH refined with riding coordinates:
 C1(H1)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C2'(H2'), C3(H3), C3'(H3'), C4(H4), C4'(H4'), C5(H5), C5'(H5')
;
_olex2_submission_special_instructions 'No special instructions were received'