A copper-phosphonate network as high-performance heterogeneous catalyst for the CO2 cycloaddition reactions and alcoholysis of epoxide
Ai, Jing; Min, Xue; Gao, Chaoying; Tian, Hong-Rui; Dang, Song; Sun, Zhong-Ming; Dalton Trans.  (2017) –; doi:10.1039/C7DT00739F

data_7042777
_publ_section_title
;
 A copper-phosphonate network as high-performance heterogeneous catalyst
 for the CO2 cycloaddition reactions and alcoholysis of epoxide
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00739F
_journal_year                    2017
_chemical_formula_moiety         '0.5(C150.22 H100 Cu14 N41.78 O56 P16 Si4)'
_chemical_formula_sum            'C75 H52 Cu7 N21 O28 P8 Si2'
_chemical_formula_weight         2444.09
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-12-22 deposited with the CCDC.
2017-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.425(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.6147(10)
_cell_length_b                   17.8396(13)
_cell_length_c                   20.1820(14)
_cell_measurement_reflns_used    3304
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.799
_cell_measurement_theta_min      2.194
_cell_volume                     4887.2(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)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.168
_diffrn_reflns_theta_min         1.873
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0704 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.8342.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_F_000             2448
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.299
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         9755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0593P)^2^+4.5524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1358
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6946
_reflns_number_total             9755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00739f2.cif
_cod_data_source_block           1_sq_s
_cod_database_code               7042777
_shelxl_version_number           2014-1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Shared sites
{C34, N34}
{C35, N35}
{C36, N36}
3. Uiso/Uaniso restraints and constraints
Uanis(C34) = Uanis(N34)
Uanis(C35) = Uanis(N35)
Uanis(C36) = Uanis(N36)
4. Others
 Sof(N34)=Sof(N35)=Sof(N36)=1-FVAR(1)
 Sof(C34)=Sof(C35)=Sof(C36)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C37(H37), C39(H39)
5.b Idealised tetrahedral OH refined as rotating group:
 O9(H9A)
;
_shelx_res_checksum              97141
_shelx_fab_checksum              7892
_olex2_submission_special_instructions 'No special instructions were received'