Synthesis of Polyynes Using Dicobalt Masking Groups.
Kohn, Daniel R.; Gawel, Przemyslaw; Xiong, Yaoyao; Christensen, Kirsten E.; Anderson, Harry L.; The Journal of organic chemistry 83 (2018) 2077–2086; doi:10.1021/acs.joc.7b03015

data_4035013
_publ_section_title
;
 Synthesis of Polyynes Using Dicobalt Masking Groups.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2077
_journal_page_last               2086
_journal_paper_doi               10.1021/acs.joc.7b03015
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C88 H86 Co4 O8 P4 Si2'
_chemical_formula_sum            'C88 H86 Co4 O8 P4 Si2'
_chemical_formula_weight         1687.44
_chemical_melting_point          ?
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2017-04-06
_audit_creation_method           CRYSTALS_ver_14.61_build_6156
_cell_angle_alpha                82.618(7)
_cell_angle_beta                 84.683(8)
_cell_angle_gamma                81.577(7)
_cell_formula_units_Z            1
_cell_length_a                   11.5368(11)
_cell_length_b                   12.2121(10)
_cell_length_c                   17.3928(18)
_cell_measurement_reflns_used    2706
_cell_measurement_temperature    100
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     2397.1(4)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Pilatus 2M'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
'Pilatus 2M detector on Crystal Logic diffractometer'
_diffrn_measurement_device_type  'Photon counting area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  Synchrotron
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.113
_diffrn_reflns_av_sigmaI/netI    0.1813
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19452
_diffrn_reflns_theta_full        20.181
_diffrn_reflns_theta_max         20.181
_diffrn_reflns_theta_min         1.645
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            clear_intense_red
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             874.000
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         5023
_refine_ls_number_restraints     820
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.0006134
_refine_ls_shift/su_mean         0.0000427
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 55.3 73.8 33.1 8.34 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1335
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1335
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                3196
_reflns_number_total             5037
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.71
_oxford_diffrn_Wilson_scale      2.72
_oxford_refine_ls_r_factor_ref   0.0881
_oxford_refine_ls_scale          0.6285(13)
_oxford_reflns_number_all        5023
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title DIA0254
_cod_data_source_file            jo7b03015_si_002.cif
_cod_data_source_block           8
_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 '_atom_sites_solution_primary' value 'Other' was changed to
'other' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/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_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4035013
_platon_squeeze_void_probe_radius 1.20