Dehydrohalogenation of proton responsive complexes: versatile aggregation via pyrazolate pincer ligand arms.
Cook, Brian J.; Chen, Chun-Hsing; Pink, Maren; Caulton, Kenneth G.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 2052–2060; doi:10.1039/c7dt04253a

data_7045288
_publ_section_title
;
 Dehydrohalogenation of proton responsive complexes: versatile aggregation
 via pyrazolate pincer ligand arms.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2052
_journal_page_last               2060
_journal_paper_doi               10.1039/c7dt04253a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C66.00 H120 Cl1 Co2 Li3 N12 O4 Si4'
_chemical_formula_sum            'C66 H120 Cl Co2 Li3 N12 O4 Si4'
_chemical_formula_weight         1432.24
_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             2017-12-15
_audit_creation_method           CRYSTALS_ver_14.61_build_6236
_audit_update_record
;
2018-01-05 deposited with the CCDC.
2018-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                63.7440(10)
_cell_angle_beta                 67.3570(10)
_cell_angle_gamma                88.2470(10)
_cell_formula_units_Z            2
_cell_length_a                   16.9176(4)
_cell_length_b                   16.9481(4)
_cell_length_c                   17.4847(4)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     4089.91(18)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.024
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33484
_diffrn_reflns_theta_full        25.230
_diffrn_reflns_theta_max         25.230
_diffrn_reflns_theta_min         1.323
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.545
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS, R. Blessing; 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.319
_exptl_crystal_size_min          0.206
_refine_diff_density_max         1.42
_refine_diff_density_min         -1.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         14535
_refine_ls_number_restraints     81
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.0281838
_refine_ls_shift/su_mean         0.0009882
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ + 8.12P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1674
_refine_ls_wR_factor_gt          0.1522
_refine_ls_wR_factor_ref         0.1673
_reflns_limit_h_max              20
_reflns_limit_h_min              -18
_reflns_limit_k_max              20
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                11596
_reflns_number_total             14603
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.64
_oxford_diffrn_Wilson_scale      183.02
_oxford_refine_ls_r_factor_ref   0.0724
_oxford_refine_ls_scale          0.11538(4)
_oxford_reflns_number_all        14538
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'mo_14027_0ma in P-1'
_cod_data_source_file            c7dt04253a2.cif
_cod_data_source_block           14027
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7045287--7045291.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C66.00 H120 Cl1 Co2 Li3 N12 O4 Si4'
_cod_database_code               7045288