A New Tri-nuclear Cu-carbonate Cluster Utilizing CO2 as C1-Building Block-Reactive Intermediates, Probable Mechanism, EPR and Magnetic Studies
Das, Biswanath; Bhadbhade, Mohan; Thapper, Anders; Ling, Chris D.; Colbran, Stephen Boyd; Dalton Transactions  (2019) –; doi:10.1039/C8DT04858D

data_7048785
_publ_section_title
;
 A New Tri-nuclear Cu-carbonate Cluster Utilizing CO2 as C1-Building
 Block-Reactive Intermediates, Probable Mechanism, EPR and Magnetic
 Studies
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT04858D
_journal_year                    2019
_chemical_formula_moiety         'C18 H24 Cu0.5 N2, B0.5 F2'
_chemical_formula_sum            'C18 H24 B0.5 Cu0.5 F2 N2'
_chemical_formula_weight         343.57
_space_group_crystal_system      trigonal
_space_group_IT_number           154
_space_group_name_Hall           'P 32 2"'
_space_group_name_H-M_alt        'P 32 2 1'
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2145p2
_audit_creation_date             2018-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-24 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   11.2232(15)
_cell_length_b                   11.2232(15)
_cell_length_c                   27.924(4)
_cell_measurement_reflns_used    6850
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      23.224
_cell_measurement_theta_min      2.188
_cell_volume                     3046.1(7)
_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    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            19079
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.987
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         2.188
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1056 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.8301. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       plate
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.045
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 1209 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3579
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0857
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1594P)^2^+2.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2253
_reflns_Friedel_coverage         0.722
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3228
_reflns_number_total             3579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04858d2.cif
_cod_data_source_block           bishwnath_10sept216_a
_cod_original_cell_volume        3046.0(9)
_cod_original_formula_sum        'C18 H24 B0.50 Cu0.50 F2 N2'
_cod_database_code               7048785
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.833
_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. Restrained distances
 F6-B0AA = F1AA-B0AA = F4AA-B0AA = F2AA-B0AA = F1-B0AA = F2-B0AA = F3AA-B0AA
 1.419 with sigma of 0.02
 F4AA-F6
 2.32 with sigma of 0.02
 F6-F3AA
 2.32 with sigma of 0.02
 F3AA-F4AA
 2.32 with sigma of 0.02
 F2AA-F1AA
 2.32 with sigma of 0.02
 F1AA-F2
 2.32 with sigma of 0.02
 F2-F2AA
 2.32 with sigma of 0.02
 F1-F4AA
 2.32 with sigma of 0.02
 F1-F6
 2.32 with sigma of 0.02
 F1-F3AA
 2.32 with sigma of 0.02
 F1-F1AA
 2.32 with sigma of 0.02
 F1-F2AA
 2.32 with sigma of 0.02
 F1-F2
 2.32 with sigma of 0.02
3. Others
 Fixed Sof: F1(0.5) F2(0.25) B0AA(0.5) F1AA(0.25) F2AA(0.25) F3AA(0.25)
 F4AA(0.25) F6(0.25)
 Fixed Uiso: F2(0.04883) F1AA(0.04883) F2AA(0.04883) F3AA(0.04883)
 F4AA(0.04883) F6(0.04883)
4.a Aromatic/amide H refined with riding coordinates:
 C006(H006), C009(H009), C00A(H00A), C00B(H00B), C00C(H00C), C00D(H00D)
4.b Idealised Me refined as rotating group:
 C00F(H00E,H00F,H00G), C00G(H00H,H00I,H00J), C00H(H00K,H00L,H00M), C00J(H00N,
 H00O,H00P), C00K(H00Q,H00R,H00S), C00L(H00T,H00U,H00V)
;
_shelx_res_checksum              39884
_olex2_submission_special_instructions 'No special instructions were received'