Conversion of CO2 from air into formate using amines and phosphorus-nitrogen PN3P-Ru(ii) pincer complexes
Guan, Chao; Pan, Yupeng; Ang, Eleanor Pei Ling; Hu, Jinsong; Yao, Changguang; Huang, Mei-Hui; Li, Huaifeng; Lai, Zhiping; Huang, Kuo-Wei; Green Chemistry 20 (2018) 4201–; doi:10.1039/C8GC02186D

data_7231244
_publ_section_title
;
 Conversion of CO2 from air into formate using amines and
 phosphorus-nitrogen PN3P-Ru(ii) pincer complexes
;
_journal_issue                   18
_journal_name_full               'Green Chemistry'
_journal_page_first              4201
_journal_paper_doi               10.1039/C8GC02186D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C48 H40 N3 O P3 Ru'
_chemical_formula_sum            'C48 H40 N3 O P3 Ru'
_chemical_formula_weight         868.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2018-03-07 deposited with the CCDC.
2018-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                106.192(4)
_cell_angle_beta                 93.516(4)
_cell_angle_gamma                106.236(4)
_cell_formula_units_Z            4
_cell_length_a                   12.2479(14)
_cell_length_b                   20.634(2)
_cell_length_c                   25.309(3)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    180
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.27
_cell_volume                     5829.8(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      180.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            140803
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.668
_diffrn_reflns_theta_min         2.058
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1406 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.8114.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.990
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         1.473
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         32645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0990
_refine_ls_R_factor_gt           0.0770
_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^)+(0.0761P)^2^+18.3029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24457
_reflns_number_total             32645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc02186d2.cif
_cod_data_source_block           cg-ph
_cod_depositor_comments
'Adding full bibliography for 7231243--7231244.cif.'
_cod_original_cell_volume        5829.8(12)
_cod_database_code               7231244
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Riding coordinates:
 Ru1(H)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C6(H6), N1(H1), C18(H18), C17(H17), C16(H16), C15(H15),
 C14(H14), C12(H12), C11(H11), C10(H10), C9(H9), C8(H8), C20(H20), C21(H21),
 C22(H22), C23(H23), C24(H24), C30(H30), C29(H29), C28(H28), C27(H27), C26(H26),
  C36(H36), C35(H35), C34(H34), C33(H33), C32(H32), C38(H38), C39(H39),
 C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48),
  N4(H4A), C56(H56), C68(H68), C60(H60), C80(H80), C81(H81), C82(H82), C83(H83),
  C84(H84), C90(H90), C51(H51), C52(H52), C96(H96), C78(H78), C53(H53),
 C59(H59), C66(H66), C94(H94), C62(H62), C92(H92), C69(H69), C58(H58), C65(H65),
  C63(H63), C95(H95), C75(H75), C77(H77), C76(H76), C87(H87), C89(H89),
 C74(H74), C57(H57), C72(H72), C93(H93), C86(H86), C64(H64), C70(H70), C71(H71),
  C88(H88)
2.c Fitted hexagon refined as free rotating group:
 C79(C80,C81,C82,C83,C84)
;
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'