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_4088757
_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         'C32 H35 Co N Na O4'
_chemical_formula_sum            'C32 H35 Co N Na O4'
_chemical_formula_weight         579.53
_chemical_melting_point          ?
_chemical_name_common            Na(Et2O)[Co(CO)3(CNArMes2)]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                104.217(8)
_cell_angle_beta                 111.985(8)
_cell_angle_gamma                90.688(8)
_cell_formula_units_Z            2
_cell_length_a                   11.2666(14)
_cell_length_b                   12.1163(14)
_cell_length_c                   12.1953(12)
_cell_measurement_reflns_used    2084
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.342
_cell_measurement_theta_min      2.885
_cell_volume                     1486.4(3)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_collection       'BRUKER Apex 2'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.975
_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  0.0326
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9483
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.113
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0557 before and 0.0333 after correction. 
The Ratio of minimum to maximum transmission is 0.7912. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.415
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0493P)^2^+0.1640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4049
_reflns_number_total             5765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00375_si_002.cif
_cod_data_source_block           jfig816_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 

2021-04-11
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C64 H70 Co2 N2 Na2 O8'
_cod_original_formula_weight         1159.06
_cod_original_formula_moiety         'C64 H70 Co2 N2 Na2 O8'
_cod_original_formula_units_Z            1
_cod_database_code               4088757
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.834
_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.a Secondary CH2 refined with riding coordinates: 
 C30(H30A,H30B), C31(H31A,H31B) 
2.b Aromatic/amide H refined with riding coordinates: 
 C7(H7), C8(H8), C9(H9), C14(H14), C17(H17), C23(H23), C26(H26) 
2.c Idealised Me refined as rotating group: 
 C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C22(H22A,H22B, 
 H22C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A, 
 H32B,H32C) 
;
_shelx_res_checksum              27840
_shelx_hkl_checksum              33106
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'