Metal complexes of 3-carboxyethyl substituted trispyrazolylborates: interactions with the ester carbonyl oxygens
Hammes, Brian S.; Luo, Xuemei; Chohan, Balwant S.; Carrano, Mary W.; Carrano, Carl J.; Journal of the Chemical Society, Dalton Transactions  (2002) 3374–; doi:10.1039/b204277k

data_7702827
_publ_section_title
;
 Metal complexes of 3-carboxyethyl substituted trispyrazolylborates:
 interactions with the ester carbonyl oxygens
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3374
_journal_paper_doi               10.1039/b204277k
_journal_year                    2002
_chemical_formula_sum            'C42 H56 B2 Cl La N12 O16'
_chemical_formula_weight         1080.96
_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_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                72.04(3)
_cell_angle_beta                 88.00(3)
_cell_angle_gamma                73.80(4)
_cell_formula_units_Z            1
_cell_length_a                   9.931(2)
_cell_length_b                   11.477(4)
_cell_length_c                   12.852(2)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.73
_cell_measurement_theta_min      4.30
_cell_volume                     1336.0(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3493
_diffrn_reflns_theta_max         22.83
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  n/a
_exptl_absorpt_correction_T_min  n/a
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/a
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.789
_refine_diff_density_min         -1.860
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.072
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         3243
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.142
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_obs          0.0588
_refine_ls_shift/esd_max         -0.208
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+15.4640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1653
_refine_ls_wR_factor_obs         0.1525
_reflns_number_observed          3156
_reflns_number_total             3247
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b204277k.txt
_cod_data_source_block           bsh71
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/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 'none' was changed to
'?' -- the value is perceived as not measured.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+15.4640P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. A new data item '_refine_ls_weighting_details'
was created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+15.4640P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1336.0(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702827