A Well-Defined Isocyano Analogue of HCo(CO)4. 2: Relative Brønsted Acidity as a Function of Isocyanide Ligation
Carpenter, Alex E.; Chan, Chinglin; Rheingold, Arnold L.; Figueroa, Joshua S.; Organometallics 35 (2016) 2319–; doi:10.1021/acs.organomet.6b00375

data_4088753
_publ_section_title
;
 A Well-Defined Isocyano Analogue of HCo(CO)4. 2: Relative Br\/onsted
 Acidity as a Function of Isocyanide Ligation
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2319
_journal_paper_doi               10.1021/acs.organomet.6b00375
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C80 H85 Co N3 Na O2'
_chemical_formula_sum            'C80 H85 Co N3 Na O2'
_chemical_formula_weight         1202.43
_chemical_melting_point          ?
_chemical_name_common            Na[Co(CNArMes2)3(CO)](Et2O)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-04-29
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                90
_cell_angle_beta                 100.868(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7522(7)
_cell_length_b                   18.5133(9)
_cell_length_c                   26.4525(14)
_cell_measurement_reflns_used    4879
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.10
_cell_measurement_theta_min      2.60
_cell_volume                     6614.0(6)
_computing_cell_refinement       'Bruker Apex 2'
_computing_data_collection       'Bruker Apex 2'
_computing_data_reduction        'Bruker Apex 2'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_av_unetI/netI     0.0906
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            47543
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.456
_diffrn_reflns_theta_min         2.771
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2008/1 (Bruker,2008) was used for absorption correction. 
wR2(int) was 0.0555 before and 0.0514 after correction. 
The Ratio of minimum to maximum transmission is 0.9279. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         12186
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0517
_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^)+(0.0459P)^2^+3.4282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1210
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7610
_reflns_number_total             12186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00375_si_002.cif
_cod_data_source_block           jfig721_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4088753
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.940
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Uiso/Uaniso restraints and constraints 
Uanis(Na1A) = Uanis(Na1) 
Uanis(C4S) = Uanis(C4SA) 
Uanis(C1SA) = Uanis(C1S) 
Uanis(C2SA) = Uanis(C2S) 
Uanis(O1S) = Uanis(O1SA) 
Uanis(C3SA) = Uanis(C3S) 
3. Rigid body (RIGU) restrains 
 Na1, Na1A 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
4. Others 
 Sof(Na1A)=Sof(O1SA)=Sof(C1SA)=Sof(H1SD)=Sof(H1SE)=Sof(H1SF)=Sof(C2SA)= 
 Sof(H2SC)=Sof(H2SD)=Sof(C3SA)=Sof(H3SC)=Sof(H3SD)=Sof(C4SA)=Sof(H4SD)= 
 Sof(H4SE)=Sof(H4SF)=1-FVAR(1) 
 Sof(Na1)=Sof(O1S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=Sof(H1SC)=Sof(C2S)=Sof(H2SA)= 
 Sof(H2SB)=Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(C4S)=Sof(H4SA)=Sof(H4SB)=Sof(H4SC)= 
 FVAR(1) 
5.a Secondary CH2 refined with riding coordinates: 
 C2S(H2SA,H2SB), C2SA(H2SC,H2SD), C3S(H3SA,H3SB), C3SA(H3SC,H3SD) 
5.b Aromatic/amide H refined with riding coordinates: 
 C7(H7), C8(H8), C9(H9), C14(H14), C17(H17), C23(H23), C26(H26), C31(H31), 
 C32(H32), C33(H33), C38(H38), C41(H41), C47(H47), C50(H50), C55(H55), C56(H56), 
  C57(H57), C62(H62), C65(H65), C71(H71), C74(H74) 
5.c Idealised Me refined as rotating group: 
 C1S(H1SA,H1SB,H1SC), C1SA(H1SD,H1SE,H1SF), C4S(H4SA,H4SB,H4SC), C4SA(H4SD, 
 H4SE,H4SF), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), 
 C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C37(H37A,H37B, 
 H37C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C49(H49A, 
 H49B,H49C), C52(H52A,H52B,H52C), C61(H61A,H61B,H61C), C64(H64A,H64B,H64C), 
 C67(H67A,H67B,H67C), C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C76(H76A,H76B, 
 H76C) 
;
_shelx_res_checksum              4930
_shelx_hkl_checksum              26923
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'