Dinitrogen binding, P4-activation and aza-Büchner ring expansions mediated by an isocyano analogue of the CpCo(CO) fragment.
Mokhtarzadeh, Charles C.; Rheingold, Arnold L.; Figueroa, Joshua S.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14561–14569; doi:10.1039/c6dt02789j

data_7039997
_publ_section_title
;
 Dinitrogen binding, P4-activation and aza-B\"uchner ring expansions
 mediated by an isocyano analogue of the CpCo(CO) fragment.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14561
_journal_page_last               14569
_journal_paper_doi               10.1039/c6dt02789j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C55 H61.56 Co N'
_chemical_formula_sum            'C55 H62 Co N'
_chemical_formula_weight         795.98
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-20
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-01 deposited with the CCDC.
2016-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.826(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.4977(15)
_cell_length_b                   10.7818(4)
_cell_length_c                   25.7877(9)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      2.32
_cell_volume                     10264.3(7)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_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  0.0551
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            66585
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.029
_diffrn_reflns_theta_min         1.968
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1105 before and 0.0482 after correction.
The Ratio of minimum to maximum transmission is 0.9102.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.030
_exptl_crystal_description       plate
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10126
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0455P)^2^+17.4722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7970
_reflns_number_total             10126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02789j2.cif
_cod_data_source_block           jfig1033
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039988--7039997.cif.
;
_cod_database_code               7039997
_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. Restrained distances
 C25B-C24
 1.54 with sigma of 0.02
 C25A-C24
 1.54 with sigma of 0.02
 C26B-C24
 1.54 with sigma of 0.02
 C26A-C24
 1.54 with sigma of 0.02
 C33B-C31
 1.54 with sigma of 0.02
 C33A-C31
 1.54 with sigma of 0.02
 C32B-C31
 1.54 with sigma of 0.02
 C31-C32A
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C25A) = Uanis(C25B)
Uanis(C26B) = Uanis(C26A)
Uanis(C21B) = Uanis(C21A)
Uanis(C33B) = Uanis(C33A)
Uanis(C32A) = Uanis(C32B)
Uanis(C20A) = Uanis(C20B)
Uanis(C21A) = Uanis(C21B)
Uanis(C26A) = Uanis(C26B)
4. Rigid body (RIGU) restrains
 C22, C30, C29, C28, C27, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H24A)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C25B)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(H24)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C25A)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=Sof(H33B)=Sof(H33C)=
 Sof(H33D)=1-FVAR(2)
 Sof(H31)=Sof(C33A)=Sof(H33A)=Sof(H33E)=Sof(H33F)=Sof(C32A)=Sof(H32A)=
 Sof(H32B)=Sof(H32C)=FVAR(2)
 Sof(H19A)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21B)=Sof(H21D)=
 Sof(H21E)=Sof(H21F)=1-FVAR(3)
 Sof(H19)=Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C20A)=Sof(H20A)=
 Sof(H20B)=Sof(H20C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C19(H19), C19(H19A), C24(H24), C24(H24A), C31(H31)
6.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C35(H35), C17(H17), C15(H15), C8(H8), C16(H16), C45(H45), C36(H36),
 C42(H42), C43(H43), C44(H44), C7(H7), C6(H6), C39(H39), C37(H37), C38(H38),
 C27(H27), C28(H28), C29(H29)
6.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C55(H55A,H55B,H55C), C51(H51A,H51B,
 H51C), C53(H53A,H53B,H53C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C21A(H21A,H21B,H21C), C20A(H20A,H20B,H20C), C26A(H26A,H26B,H26C), C33A(H33A,
 H33E,H33F), C25A(H25A,H25B,H25C), C32A(H32A,H32B,H32C), C26B(H26D,H26E,H26F),
 C25B(H25D,H25E,H25F), C32B(H32D,H32E,H32F), C33B(H33B,H33C,H33D), C20B(H20D,
 H20E,H20F), C21B(H21D,H21E,H21F)
;
_shelx_res_checksum              73950
_shelx_fab_checksum              56755
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'