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_4088754
_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         'C64 H74 Co N2 Na O5'
_chemical_formula_sum            'C64 H74 Co N2 Na O5'
_chemical_formula_weight         1033.17
_chemical_melting_point          ?
_chemical_name_common            Na(THF)3[Na(CO)2(CNArMes2)2]
_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     iterative
_audit_creation_date             2015-04-07
_audit_creation_method
; 
Olex2 1.2 
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) 
;
_cell_angle_alpha                75.175(9)
_cell_angle_beta                 78.801(7)
_cell_angle_gamma                68.362(7)
_cell_formula_units_Z            2
_cell_length_a                   12.5478(19)
_cell_length_b                   13.359(2)
_cell_length_c                   18.742(3)
_cell_measurement_reflns_used    9843
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.53
_cell_volume                     2805.6(8)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            48620
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.491
_diffrn_reflns_theta_min         1.131
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.1224 before and 0.0413 after correction. 
The Ratio of minimum to maximum transmission is 0.9328. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         13999
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0399P)^2^+1.3241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11191
_reflns_number_total             13999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00375_si_002.cif
_cod_data_source_block           jfig819_1_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_original_cell_volume        2805.5(8)
_cod_database_code               4088754
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.839
_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(C2SB) = Uanis(C2SA) 
Uanis(C1SB) = Uanis(C1SA) 
3. Rigid body (RIGU) restrains 
 C2SB, C2SA, C1SB, C1SA, C4SB, C4SA, C3SB, C3SA 
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 
4. Others 
 Sof(C1SB)=Sof(H1SA)=Sof(H1SB)=Sof(C2SB)=Sof(H2SA)=Sof(H2SB)=Sof(C3SB)= 
 Sof(H3SA)=Sof(H3SB)=Sof(C4SB)=Sof(H4SA)=Sof(H4SB)=1-FVAR(1) 
 Sof(C4SA)=Sof(H4SC)=Sof(H4SD)=Sof(C3SA)=Sof(H3SC)=Sof(H3SD)=Sof(C2SA)= 
 Sof(H2SC)=Sof(H2SD)=Sof(C1SA)=Sof(H1SC)=Sof(H1SD)=FVAR(1) 
5.a Secondary CH2 refined with riding coordinates: 
 C1SB(H1SA,H1SB), C2SB(H2SA,H2SB), C3SB(H3SA,H3SB), C4SB(H4SA,H4SB), C53(H53A, 
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), 
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C4SA(H4SC,H4SD), C3SA(H3SC, 
 H3SD), C2SA(H2SC,H2SD), C1SA(H1SC,H1SD) 
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) 
5.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), C37(H37A,H37B,H37C), C40(H40A, 
 H40B,H40C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), 
 C52(H52A,H52B,H52C) 
;
_shelx_res_checksum              76007
_shelx_hkl_checksum              14717
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'