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_7020576
_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         'C64 H46 Fe1 N8 O4'
_chemical_formula_sum            'C64 H46 Fe N8 O4'
_chemical_formula_weight         1046.97
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             12-04-17
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 95.0494(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.8206(2)
_cell_length_b                   12.3235(2)
_cell_length_c                   15.5858(2)
_cell_measurement_reflns_used    6964
_cell_measurement_temperature    150
_cell_measurement_theta_max      29
_cell_measurement_theta_min      5
_cell_volume                     2644.24(7)
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.020
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58363
_diffrn_reflns_theta_full        28.027
_diffrn_reflns_theta_max         28.599
_diffrn_reflns_theta_min         5.134
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            clear_pale_green
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9298
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6705
_refine_ls_number_restraints     256
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.0034395
_refine_ls_shift/su_mean         0.0001825
_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:
17.8 26.3 12.6 3.22
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0941
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.0941
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                5355
_reflns_number_total             6705
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.22
_oxford_diffrn_Wilson_scale      4.88
_oxford_refine_ls_r_factor_ref   0.0516
_oxford_refine_ls_scale          0.4405(4)
_oxford_reflns_number_all        6705
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 014mwj12
_cod_data_source_file            c2dt31859h.txt
_cod_data_source_block           15
_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.

'_atom_sites_solution_primary'
value 'Other' changed to 'other' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

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/c '
_cod_original_formula_sum        'C64 H46 Fe1 N8 O4'
_cod_database_code               7020576
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 1,X'S) H ( 11,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
SAME C(20) C(27) C(28) C(29) C(30) C(31) C(32) AND
CONT C(20) C(27) C(32) C(31) C(30) C(29) C(28) AND
CONT C(20) C(33) C(34) C(35) C(36) C(37) C(38) AND
CONT C(20) C(33) C(38) C(37) C(36) C(35) C(34)
SIMU 0.01 C(20) C(27) C(28) C(29) C(30) C(31) C(32) AND
CONT C(20) C(27) C(32) C(31) C(30) C(29) C(28) AND
CONT C(20) C(33) C(34) C(35) C(36) C(37) C(38) AND
CONT C(20) C(33) C(38) C(37) C(36) C(35) C(34)
DELU 0.01 C(20) C(27) C(28) C(29) C(30) C(31) C(32) AND
CONT C(20) C(27) C(32) C(31) C(30) C(29) C(28) AND
CONT C(20) C(33) C(34) C(35) C(36) C(37) C(38) AND
CONT C(20) C(33) C(38) C(37) C(36) C(35) C(34)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;