Dimerization of terminal alkynes promoted by a heterobimetallic Zr/Co complex.
Beattie, Jeffrey W.; Wang, Canning; Zhang, Hongtu; Krogman, Jeremy P.; Foxman, Bruce M.; Thomas, Christine M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2407–2411; doi:10.1039/d0dt00334d

data_7703416
_publ_section_title
;
 Dimerization of terminal alkynes promoted by a heterobimetallic Zr/Co
 complex.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2407
_journal_page_last               2411
_journal_paper_doi               10.1039/d0dt00334d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C61 H87 Co1 N3 P3 Zr1'
_chemical_formula_sum            'C61 H87 Co N3 P3 Zr'
_chemical_formula_weight         1105.46
_chemical_melting_point          ?
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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     direct
_audit_creation_date             2019-11-12
_audit_creation_method           'CRYSTALS_ver_14.61_build_7408 '
_audit_update_record
;
2019-11-13 deposited with the CCDC.	2020-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.923(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0196(9)
_cell_length_b                   34.104(3)
_cell_length_c                   13.9512(9)
_cell_measurement_reflns_used    1992
_cell_measurement_temperature    120
_cell_measurement_theta_max      21.90
_cell_measurement_theta_min      2.39
_cell_volume                     5664.2(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.127
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            37487
_diffrn_reflns_theta_full        23.077
_diffrn_reflns_theta_max         23.077
_diffrn_reflns_theta_min         1.194
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             2344
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: diethyl ether'
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.29
_refine_diff_density_min         -1.22
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         7966
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.0010878
_refine_ls_shift/su_mean         0.0000371
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 4.42P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0912
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0912
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              37
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4927
_reflns_number_total             7966
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.1064
_oxford_refine_ls_scale          0.083157(13)
_oxford_reflns_number_all        7966
_oxford_structure_analysis_title 'JK_320_0m in P2(1)/n'
_cod_data_source_file            d0dt00334d2.cif
_cod_data_source_block           2a
_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 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7703415--7703416.cif.
;
_cod_original_cell_volume        5664.3(7)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C61 H87 Co1 N3 P3 Zr1'
_cod_database_code               7703416
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)