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_7039993
_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         'C72 H89 Co N2, C2 H3.5 O0.5'
_chemical_formula_sum            'C74 H92 Co N2 O0.5'
_chemical_formula_weight         1077.5
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-31
_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                 96.131(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.222(3)
_cell_length_b                   14.0788(17)
_cell_length_c                   21.829(3)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.41
_cell_volume                     6484.8(15)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0732
_diffrn_reflns_av_unetI/netI     0.0887
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            46172
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.384
_diffrn_reflns_theta_max         25.384
_diffrn_reflns_theta_min         1.739
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.3617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1629 before and 0.0756 after correction.
The Ratio of minimum to maximum transmission is 0.4854.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         11825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0518P)^2^+2.0755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8566
_reflns_number_total             11825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02789j2.cif
_cod_data_source_block           jfig1026
_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_original_cell_volume        6484.6(14)
_cod_database_code               7039993
_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. Others
 Fixed Sof: H72A(0.5) H72B(0.5) H72C(0.5) C73A(0.5) H73A(0.5) H73B(0.5)
 C73B(0.5) H73C(0.5) H73D(0.5)
3.a Ternary CH refined with riding coordinates:
 C48(H48), C53(H53), C30(H30), C18(H18), C41(H41), C60(H60), C11(H11), C23(H23)
3.b Secondary CH2 refined with riding coordinates:
 C73A(H73A,H73B), C73B(H73C,H73D)
3.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C6(H6), C36(H36), C16(H16), C7(H7), C58(H58), C5(H5), C28(H28),
 C35(H35), C56(H56), C26(H26), C14(H14), C57(H57), C15(H15), C27(H27), C46(H46),
  C45(H45), C44(H44)
3.d Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C62(H62A,H62B,H62C), C65(H65A,H65B,
 H65C), C42(H42A,H42B,H42C), C31(H31A,H31B,H31C), C13(H13A,H13B,H13C), C19(H19A,
 H19B,H19C), C32(H32A,H32B,H32C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C),
 C50(H50A,H50B,H50C), C67(H67A,H67B,H67C), C71(H71A,H71B,H71C), C43(H43A,H43B,
 H43C), C63(H63A,H63B,H63C), C69(H69A,H69B,H69C), C25(H25A,H25B,H25C), C49(H49A,
 H49B,H49C), C61(H61A,H61B,H61C), C12(H12A,H12B,H12C), C72(H72A,H72B,H72C)
;
_shelx_res_checksum              17560
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'