Unusual cyanide and methyl binding modes at a dicobalt macrocycle following acetonitrile C-C bond activation.
Spentzos, Ariana Z.; Gau, Michael R.; Carroll, Patrick J.; Tomson, Neil C.; Chemical communications (Cambridge, England) 56 (2020) 9675–9678; doi:10.1039/d0cc03521a

data_7126890
_publ_section_title
;
 Unusual cyanide and methyl binding modes at a dicobalt macrocycle
 following acetonitrile C-C bond activation.
;
_journal_issue                   67
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9675
_journal_page_last               9678
_journal_paper_doi               10.1039/d0cc03521a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C39 H64 Co2 N7 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C41 H64 Co2 F6 N7 O6 P2 S2'
_chemical_formula_weight         1108.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2020-05-06 deposited with the CCDC.	2020-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_diffrn_ambient_environment      N~2~
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_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -23.00  39.00   0.50    2.00    --    5.07 -99.00 150.00  124
  2  \w    -23.00  39.00   0.50    2.00    --    5.07 -99.00 120.00  124
  3  \w    -69.00  29.00   0.50    2.00    --    5.07 -77.00  60.00  196
  4  \w     -8.00  30.00   0.50    2.00    --    5.07 -99.00  30.00   76
  5  \w     -2.00  27.00   0.50    2.00    --    5.07 -99.00 -90.00   58
  6  \w     -3.00  79.00   0.50    2.00    --    5.07  77.00 150.00  164
  7  \w    -11.00  78.00   0.50    2.00    --    5.07  57.00   0.00  178
  8  \w    -12.00  26.00   0.50    2.00    --   -5.38 -99.00-150.00   76
  9  \w    -18.00   8.00   0.50    2.00    --   -5.38 -99.00 -90.00   52
 10  \w    -84.00 -44.00   0.50    2.00    --   -5.38 178.00  90.00   80
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0151797000
_diffrn_orient_matrix_UB_12      -0.0007748000
_diffrn_orient_matrix_UB_13      0.0365842000
_diffrn_orient_matrix_UB_21      0.0077409000
_diffrn_orient_matrix_UB_22      0.0558480000
_diffrn_orient_matrix_UB_23      -0.0003668000
_diffrn_orient_matrix_UB_31      -0.0322010000
_diffrn_orient_matrix_UB_32      0.0130687000
_diffrn_orient_matrix_UB_33      0.0037452000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            45191
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.092
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       plank
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.043
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5619
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0499P)^2^+14.1078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                5073
_reflns_number_total             5619
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           3727
_cod_depositor_comments
'Adding full bibliography for 7126890--7126893.cif.'
_cod_original_cell_volume        4904.9(2)
_cod_database_code               7126890
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_digest_frames
;
01215ac70129d5678a1330bc7b83de00af01128a0b5
;
_diffrn_oxdiff_digest_hkl
;
01166b3fab8d42054df58178e9c00e298fd9d1
;
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42