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_7048784
_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 Cl2 Cu N2, 1(B F4), C6 H16 N'
_chemical_formula_sum            'C24 H40 B Cl2 Cu F4 N3'
_chemical_formula_weight         591.84
_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_block_doi                 10.5517/ccdc.csd.cc2145n1
_audit_creation_date             2016-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2018-11-23 deposited with the CCDC.
2019-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                86.824(4)
_cell_angle_beta                 81.552(4)
_cell_angle_gamma                81.251(4)
_cell_formula_units_Z            2
_cell_length_a                   7.4731(5)
_cell_length_b                   13.2115(10)
_cell_length_c                   14.9811(11)
_cell_measurement_reflns_used    8117
_cell_measurement_temperature    221.99
_cell_measurement_theta_max      26.116
_cell_measurement_theta_min      2.751
_cell_volume                     1445.20(18)
_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)'
_diffrn_ambient_temperature      221.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0595
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30697
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.062
_diffrn_reflns_theta_min         2.751
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1297 before and 0.0695 after correction.
The Ratio of minimum to maximum transmission is 0.9084.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'bluish green'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       plate
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6317
_refine_ls_number_restraints     149
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0569P)^2^+0.6322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4822
_reflns_number_total             6317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04858d2.cif
_cod_data_source_block           crystal2_cu_a
_cod_database_code               7048784
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2T-C1T \\sim C2T'-C1T
 with sigma of 0.02
 C4T'-C3T \\sim C4T-C3T
 with sigma of 0.02
 C6T-C5T \\sim C6T'-C5T
 with sigma of 0.02
 F4A-F3A \\sim F4A-F1A \\sim F3A-F1A \\sim F3A-F2A \\sim F1A-F2A
 with sigma of 0.04
 B1-F4A \\sim B1-F3A \\sim B1-F1A \\sim B1-F2A
 with sigma of 0.02
 F1-F2 \\sim F1-F5 \\sim F1-F0AA \\sim F2-F5 \\sim F5-F0AA
 with sigma of 0.04
 B11-F1 \\sim B11-F2 \\sim B11-F5 \\sim B11-F0AA
 with sigma of 0.02
 B2-F2AA \\sim B2-F4 \\sim B2-F4A \\sim B2-F1AA
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(B2) = Uanis(B1) = Uanis(B11)
4. Rigid body (RIGU) restrains
 C5T, C6T'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5T, C6T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1T, C2T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2T', C1T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3T, C4T
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3T, C4T'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B1, F3AA, F2A, F3A, F1A, B2, F4A, F2AA, F1AA, F4, B11, F1, F5, F2, F0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: B1(0.33333) H1TC(0.5) H1TD(0.5) H1TA(0.5) H1TB(0.5) C2T(0.5)
 H2TA(0.5) H2TB(0.5) H2TC(0.5) H3TA(0.5) H3TB(0.5) H3TC(0.5) H3TD(0.5) C4T(0.5)
 H4TA(0.5) H4TB(0.5) H4TC(0.5) H5TC(0.5) H5TD(0.5) H5TA(0.5) H5TB(0.5) C6T(0.5)
 H6TA(0.5) H6TB(0.5) H6TC(0.5) C2T'(0.5) H2TD(0.5) H2TE(0.5) H2TF(0.5)
 C4T'(0.5) H4TD(0.5) H4TE(0.5) H4TF(0.5) C6T'(0.5) H6TD(0.5) H6TE(0.5)
 H6TF(0.5) F4A(0.33333) F3A(0.33333) F1A(0.33333) F2A(0.33333) F1(0.33333)
 F2(0.33333) F5(0.33333) F0AA(0.33333) B11(0.33333) B2(0.33333) F1AA(0.33333)
 F2AA(0.33333) F4(0.33333) F3AA(0.33333)
6.a Ternary CH refined with riding coordinates:
 N1T(H1T)
6.b Secondary CH2 refined with riding coordinates:
 C1T(H1TC,H1TD), C1T(H1TA,H1TB), C3T(H3TA,H3TB), C3T(H3TC,H3TD), C5T(H5TC,
 H5TD), C5T(H5TA,H5TB)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C9(H9), C10(H10)
6.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C2T(H2TA,H2TB,H2TC), C4T(H4TA,
 H4TB,H4TC), C6T(H6TA,H6TB,H6TC), C2T'(H2TD,H2TE,H2TF), C4T'(H4TD,H4TE,H4TF),
 C6T'(H6TD,H6TE,H6TF)
;
_shelx_res_checksum              94992
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'