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_4088755
_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         'C52 H50 Co N2 O2, C36 H30 N P2, C4 H10 O'
_chemical_formula_sum            'C92 H90 Co N3 O3 P2'
_chemical_formula_weight         1406.53
_chemical_melting_point          ?
_chemical_name_common            'PPN[Co(CO)2(CNArMes2)2] Et2O'
_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     direct
_audit_creation_date             2016-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.267(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.377(4)
_cell_length_b                   16.575(3)
_cell_length_c                   38.687(6)
_cell_measurement_reflns_used    5462
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.50
_cell_volume                     15469(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.85
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_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  0.1341
_diffrn_reflns_av_unetI/netI     0.1453
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            53951
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_min         1.491
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0788 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.8359.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5952
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     918
_refine_ls_number_reflns         14088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.1836
_refine_ls_R_factor_gt           0.1056
_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^)+(0.0033P)^2^+204.8746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8111
_reflns_number_total             14088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00375_si_002.cif
_cod_data_source_block           jfig405
_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               4088755
_shelx_estimated_absorpt_t_max   0.940
_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(C7C) = Uanis(C1C)
3.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C3S(H3SA,H3SB)
3.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), 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(H16D), C17C(H17C), C18C(H18C),
 C20C(H20C), C21C(H21C), C22C(H22D), C23C(H23C), C24C(H24C), C26C(H26C),
 C27C(H27C), C28C(H28D), C29C(H29C), C30C(H30C), C33C(H33C), C34C(H34C),
 C35C(H35C), C36C(H36C), C37C(H37D)
3.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), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              85321
_shelx_hkl_checksum              33127
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'