Synthesis of new bulky bis(pyrazolyl)methane carboxylate (heteroscorpionate) ligands and their complexes with iron, manganese and nickel.
Jones, Michael W.; Baldwin, Jack E.; Cowley, Andrew R.; Dilworth, Jonathan R.; Karpov, Alexei; Smiljanic, Nicolas; Thompson, Amber L.; Adlington, Robert M.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 14068–14086; doi:10.1039/c2dt31859h

data_7020585
_publ_section_title
;
 Synthesis of new bulky bis(pyrazolyl)methane carboxylate
 (heteroscorpionate) ligands and their complexes with iron, manganese and
 nickel.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14068
_journal_page_last               14086
_journal_paper_doi               10.1039/c2dt31859h
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C108 H96 Fe N15 O18, 2(C4 H10 O), C H2 Cl2'
_chemical_formula_sum            'C117 H118 Cl2 Fe N15 O20'
_chemical_formula_weight         2181.07
_chemical_melting_point          ?
_space_group_IT_number           14
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-07-02
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                90
_cell_angle_beta                 92.4789(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2222(4)
_cell_length_b                   23.5384(5)
_cell_length_c                   23.4924(5)
_cell_measurement_reflns_used    20180
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     11171.9(4)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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      150
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.152
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            95334
_diffrn_reflns_theta_full        25.372
_diffrn_reflns_theta_max         25.372
_diffrn_reflns_theta_min         5.114
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_intense_orange
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4579.999
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.69
_refine_diff_density_min         -0.98
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9920
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         10056
_refine_ls_number_restraints     973
_refine_ls_R_factor_all          0.2089
_refine_ls_R_factor_gt           0.1212
_refine_ls_shift/su_max          0.0011963
_refine_ls_shift/su_mean         4.7438626
_refine_ls_structure_factor_coef F
_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:
-1.23 -3.10 -1.86 -0.989
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0881
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0577
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                10056
_reflns_number_total             20309
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.93
_oxford_diffrn_Wilson_scale      150.03
_oxford_refine_ls_r_factor_ref   0.1212
_oxford_refine_ls_scale          0.09397(18)
_oxford_reflns_number_all        20309
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 6104
_cod_data_source_file            c2dt31859h.txt
_cod_data_source_block           32
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C117 H118 Cl2 Fe1 N15 O20'
_cod_database_code               7020585