Chelated [Zn(cyclam)]2+ Lewis Acid Improves the Reactivity of the Electrochemical Reduction of CO2 by Mn Catalysts with Bulky Bipyridine Ligands
Zhanaidarova, Almagul; Steger, Han; Reineke, Mark H.; Kubiak, Clifford P.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02620J

data_7044010
_publ_section_title
;
 Chelated [Zn(cyclam)]2+ Lewis Acid Improves the Reactivity of the
 Electrochemical Reduction of CO2 by Mn Catalysts with Bulky Bipyridine
 Ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02620J
_journal_year                    2017
_chemical_compound_source        n/a
_chemical_formula_moiety         'C14 H30 N6 Zn, 2(B F4)'
_chemical_formula_sum            'C14 H30 B2 F8 N6 Zn'
_chemical_formula_weight         521.43
_chemical_melting_point          200
_chemical_name_common            'Zinc cyclam tetrafluoroborate'
_chemical_name_systematic        '[Zn(cyclam)(2MeCN)](BF4)2'
_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
_audit_creation_date             2017-07-17
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.07.14 svn.r3447 for OlexSys, GUI svn.r5367)
;
_audit_update_record
;
2017-07-17 deposited with the CCDC.
2017-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.5920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4835(5)
_cell_length_b                   7.9463(2)
_cell_length_c                   18.0503(5)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.188
_cell_measurement_theta_min      5.566
_cell_volume                     2280.25(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Platinum135 CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Platinum135'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            36573
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         68.268
_diffrn_reflns_theta_min         2.957
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Rigaku MicroMax-007HF'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.223
_exptl_absorpt_correction_T_max  0.5210
_exptl_absorpt_correction_T_min  0.4233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0711 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.8125. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            Colorless
_exptl_crystal_colour_primary    Colorless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       Block
_exptl_crystal_F_000             1072
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeCN, Et2O'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         4171
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0358P)^2^+2.0229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0781
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3847
_reflns_number_total             4171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02620j2.cif
_cod_data_source_block           p21n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7044010
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F00O-B00U \\sim F00P-B00U \\sim F00S-B00U \\sim F00T-B00U \\sim F00V-B00U
\\sim F00W-B00U
 with sigma of 0.003
3. Rigid body (RIGU) restrains
 B00U, F005, F00O, F00S, F00V, F00T, F00P, F00W
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F00T)=Sof(F00P)=Sof(F00W)=1-FVAR(1)
 Sof(F00O)=Sof(F00S)=Sof(F00V)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N006(H006), N008(H008), N009(H009), N00A(H00A)
5.b Secondary CH2 refined with riding coordinates:
 C00F(H00B,H00C), C00G(H00D,H00E), C00H(H00F,H00G), C00I(H00H,H00I), C00J(H00J,
 H00K), C00K(H00L,H00M), C00L(H00N,H00O), C00M(H00P,H00Q), C00N(H00R,H00S),
 C00P(H00T,H00U)
5.c Idealised Me refined as rotating group:
 C00Q(H00V,H00W,H00X), C00R(H00Y,H,HA)
;
_shelx_res_checksum              51772
_olex2_submission_special_instructions 'No special instructions were received'