Fixation of atmospheric CO<sub>2</sub> as C1-feedstock by nickel(ii) complexes.
Muthuramalingam, Sethuraman; Velusamy, Marappan; Mayilmurugan, Ramasamy; Dalton transactions (Cambridge, England : 2003) 50 (2021) 7984–7994; doi:10.1039/d0dt03887c

data_7707194
_publ_section_title
;
 Fixation of atmospheric CO<sub>2</sub> as C1-feedstock by nickel(ii)
 complexes.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7984
_journal_page_last               7994
_journal_paper_doi               10.1039/d0dt03887c
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H54 N6 Ni2 O7, 2(Cl O4), C3 H6 O, 2(H2 O)'
_chemical_formula_sum            'C34 H64 Cl2 N6 Ni2 O18'
_chemical_formula_weight         1033.23
_chemical_name_common
'(mu2-carbonatato)-diaqua-bis(1-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-4-methyl-1,4-diazepane-N,N',N")-di-nickel(II) diperchlorate acetone solvate dihydrate'
_chemical_name_systematic
'(mu2-carbonatato)-diaqua-bis(1-[(4-methoxy-3,5-dimethylpyridin-2-yl)methyl]-4-methyl-1,4-diazepane-N,N',N")-di-nickel(II) diperchlorate acetone solvate dihydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_audit_update_record
;
2021-04-23 deposited with the CCDC.	2021-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7462(7)
_cell_length_b                   15.1861(9)
_cell_length_c                   25.9560(16)
_cell_measurement_reflns_used    3853
_cell_measurement_temperature    290.9(4)
_cell_measurement_theta_max      28.570
_cell_measurement_theta_min      3.985
_cell_volume                     4630.0(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      290.9(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0640
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  23.00   0.50    3.40    --  -17.74 -99.00 120.00   96
  2  \w    -49.00  50.00   0.50    3.40    --   20.09 -77.00-150.00  198
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            13024
_diffrn_reflns_point_group_measured_fraction_full 0.899
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         3.414
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.613
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 2513 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.025(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         9085
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0636P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.649
_reflns_Friedel_fraction_full    0.793
_reflns_Friedel_fraction_max     0.793
_reflns_number_gt                7600
_reflns_number_total             9085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03887c2.cif
_cod_data_source_block           MU4a
_cod_depositor_comments
'Adding full bibliography for 7707193--7707196.cif.'
_cod_database_code               7707194
_shelx_estimated_absorpt_t_min   0.880
_shelx_estimated_absorpt_t_max   0.924
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelxl_version_number           2014/6
_shelx_res_checksum              10791