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_4035014
_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 H87 Co4 O8 P4 Si2'
_chemical_formula_sum            'C88 H87 Co4 O8 P4 Si2'
_chemical_formula_weight         1688.45
_chemical_melting_point          ?
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 98.528(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4102(5)
_cell_length_b                   16.2137(7)
_cell_length_c                   37.474(2)
_cell_measurement_reflns_used    9331
_cell_measurement_temperature    100
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     8658.7(7)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'Diamond GDA'
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.170
_diffrn_reflns_av_sigmaI/netI    0.2427
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            65669
_diffrn_reflns_theta_full        20.200
_diffrn_reflns_theta_max         20.200
_diffrn_reflns_theta_min         1.556
_diffrn_source                   Synchrotron
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3500
_exptl_crystal_size_max          0.035
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.006
_refine_diff_density_max         0.97
_refine_diff_density_min         -0.65
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1068
_refine_ls_number_reflns         6963
_refine_ls_number_restraints     226
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.0006396
_refine_ls_shift/su_mean         0.0000352
_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: 
 173. 247. 141. 52.4 8.29 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1529
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1529
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              37
_reflns_limit_l_min              0
_reflns_number_gt                4394
_reflns_number_total             9109
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.34
_oxford_diffrn_Wilson_scale      7.31
_oxford_refine_ls_r_factor_ref   0.0976
_oxford_refine_ls_scale          0.4878(9)
_oxford_reflns_number_all        6963
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title DIA0256
_cod_data_source_file            jo7b03015_si_002.cif
_cod_data_source_block           8b
_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 21/n '
_cod_database_code               4035014
_platon_squeeze_void_probe_radius 1.20