Copper(i) iodide cluster-based lanthanide organic frameworks: synthesis and application as efficient catalysts for carboxylative cyclization of propargyl alcohols with CO<sub>2</sub> under mild conditions.
Wu, Zhilei; Lan, Xingwang; Zhang, Yaxin; Li, Meng; Bai, Guoyi; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11063–11069; doi:10.1039/c9dt01859j

data_7700293
_publ_section_title
;
 Copper(i) iodide cluster-based lanthanide organic frameworks: synthesis
 and application as efficient catalysts for carboxylative cyclization of
 propargyl alcohols with CO<sub>2</sub> under mild conditions.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11063
_journal_page_last               11069
_journal_paper_doi               10.1039/c9dt01859j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'C48 H52 Cu2 Gd2 I2 N10 O16, 4(C3 H7 N O), 0.5(C6 N2 O2)'
_chemical_formula_sum            'C63 H80 Cu2 Gd2 I2 N15 O21'
_chemical_formula_weight         2078.80
_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   geom
_audit_creation_date             2018-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-05 deposited with the CCDC.    2019-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                65.919(2)
_cell_angle_beta                 86.020(2)
_cell_angle_gamma                82.341(2)
_cell_formula_units_Z            1
_cell_length_a                   12.9904(5)
_cell_length_b                   13.0609(5)
_cell_length_c                   13.4710(6)
_cell_measurement_reflns_used    9799
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.27
_cell_volume                     2067.76(15)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30167
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.198
_exptl_absorpt_coefficient_mu    2.910
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6194
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0721 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.8310.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1023
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.254
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         7290
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+1.5986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5735
_reflns_number_total             7290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01859j2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7700292--7700293.cif.'
_cod_database_code               7700293
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.740
_shelx_estimated_absorpt_t_min   0.456
_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. Uiso/Uaniso restraints and constraints
Uanis(C33) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
3. Others
 Fixed Sof: O11(0.5) C32(0.5) C31(0.5) C33(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C5(H5), C3(H3), C6(H6), C7(H7), C4(H4), C22(H22), C15(H15),
 C11(H11), C8(H8), C18(H18), C10(H10), C16(H16), C17(H17), C28(H28), C25(H25)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              11375
_olex2_submission_special_instructions 'No special instructions were received'