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_4088758
_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         'C28 H25 Co N O3, C36 H30 N P2, C6 H5 F'
_chemical_formula_sum            'C70 H60 Co F N2 O3 P2'
_chemical_formula_weight         1117.07
_chemical_melting_point          ?
_chemical_name_common            PPN[Co(CNArMes2)(CO)3]
_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
_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                106.515(2)
_cell_angle_beta                 96.958(3)
_cell_angle_gamma                96.827(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5064(7)
_cell_length_b                   15.3040(8)
_cell_length_c                   16.2449(9)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.355
_cell_measurement_theta_min      2.205
_cell_volume                     2920.4(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            36934
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.506
_diffrn_reflns_theta_min         1.406
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6360
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1319 before and 0.0517 after correction.
The Ratio of minimum to maximum transmission is 0.8535.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_preparation       'crystalized form C6H5F and pentane at -40C'
_exptl_crystal_size_max          1.079
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.113
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         10440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0263P)^2^+2.0061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8411
_reflns_number_total             10440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00375_si_002.cif
_cod_data_source_block           jfig962_0m_a
_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 '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

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               4088758
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.671
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C23(H23), C26(H26), C14(H14), C17(H17), C2C(H2C),
 C3C(H3C), C4C(H4C), C5C(H5C), C6C(H6C), C8C(H8C), C9C(H9C), C10C(H10C),
 C11C(H11C), C12C(H12C), C14C(H14C), C15C(H15C), C16C(H16C), C17C(H17C),
 C18C(H18C), C20C(H20C), C21C(H21C), C22C(H22C), C23C(H23C), C24C(H24C),
 C26C(H26C), C27C(H27C), C28C(H28C), C29C(H29C), C30C(H30C), C32C(H32C),
 C33C(H33C), C34C(H34C), C35C(H35C), C36C(H36C), C3S(H3S), C4S(H4S), C2S(H2S),
 C5S(H5S), C6S(H6S)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22D), C24(H24A,H24B,H24D), C28(H28A,H28B,H28D), C13(H13A,H13B,
 H13C), C16(H16A,H16B,H16D), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              88130
_shelx_hkl_checksum              97626
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'