Rational design of carborane-based Cu2-paddle wheel coordination polymers for increased hydrolytic stability
Li, Zhen; Choquesillo-Lazarte, Duane; Fraile, Julio; Viñas, Clara; Teixidor, Francesc; Planas, José G.; Dalton Transactions  (2022) –; doi:10.1039/D1DT04065K

data_7709170
_publ_section_title
;
 Rational design of carborane-based Cu2-paddle wheel coordination polymers
 for increased hydrolytic stability
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04065K
_journal_year                    2022
_chemical_formula_moiety         'C33 H41 B20 Cu2 O10, 1[C4H9NO]'
_chemical_formula_sum            'C37 H50 B20 Cu2 N O11'
_chemical_formula_weight         1028.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-04-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-11-02 deposited with the CCDC.	2021-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.957(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.912(4)
_cell_length_b                   7.1244(9)
_cell_length_c                   28.323(4)
_cell_measurement_reflns_used    2630
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      60.69
_cell_measurement_theta_min      3.18
_cell_volume                     5104.3(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1742
_diffrn_reflns_av_unetI/netI     0.1349
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46727
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.423
_diffrn_reflns_theta_max         66.423
_diffrn_reflns_theta_min         6.212
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1089 before and 0.0945 after correction.
The Ratio of minimum to maximum transmission is 0.7426.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         8905
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0942P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.2078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4214
_reflns_number_total             8905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04065k2.cif
_cod_data_source_block           ZLLMF3_CuP
_cod_original_cell_volume        5104.4(12)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7709170
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.844
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 C2-H1
 1.932277 with sigma of 0.02
 Cu1-H1
 2.805997 with sigma of 0.02
3. Rigid bond restraints
 O1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
5. Rigid body (RIGU) restrains
 O1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
6.a Free rotating group:
 O1(H1,C2)
6.b Rotating group:
 O2(H2D,H2E)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C17(H17), C18(H18), C23(H23), C25(H25), C26(H26),
 C27(H27), C44(H44), C46(H46), C47(H47), C48(H48), C53(H53), C55(H55), C56(H56),
  C57(H57)
6.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
6.e Boron cage BH refined with riding coordinates:
 B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B8(H8), B9(H9), B10(H10), B11(H11),
 B12(H12), B32(H32), B33(H33), B34(H34), B35(H35), B36(H36), B38(H38), B39(H39),
  B41(H41), B42(H42)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              81224
_shelx_fab_checksum              86985
_olex2_submission_special_instructions 'No special instructions were received'