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_7020579
_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         'C88 H94 Fe N8 O12, 2(C H2 Cl2)'
_chemical_formula_sum            'C90 H98 Cl4 Fe N8 O12'
_chemical_formula_weight         1681.47
_chemical_melting_point          ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-02-16
_audit_creation_method           CRYSTALS_ver_14.18
_cell_angle_alpha                80.272(3)
_cell_angle_beta                 66.147(4)
_cell_angle_gamma                85.055(3)
_cell_formula_units_Z            1
_cell_length_a                   12.5703(5)
_cell_length_b                   13.0224(5)
_cell_length_c                   14.5998(6)
_cell_measurement_reflns_used    8705
_cell_measurement_temperature    150
_cell_measurement_theta_max      76
_cell_measurement_theta_min      3
_cell_volume                     2153.94(16)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22779
_diffrn_reflns_theta_full        73.603
_diffrn_reflns_theta_max         75.879
_diffrn_reflns_theta_min         3.346
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.071
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies (Oxford Diffraction, 2002),
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            clear_pale_yellow
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.48
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0007
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8891
_refine_ls_number_restraints     68
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.0038675
_refine_ls_shift/su_mean         0.0000839
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 1.29P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1234
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1233
_reflns_limit_h_max              15
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7313
_reflns_number_total             8892
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.81
_oxford_diffrn_Wilson_scale      0.09
_oxford_refine_ls_r_factor_ref   0.0544
_oxford_refine_ls_scale          3.80(4)
_oxford_reflns_number_all        8892
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 037mwj10/6328
_cod_data_source_file            c2dt31859h.txt
_cod_data_source_block           18
_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.

'_symmetry_cell_setting' value
'Triclinic' changed to 'triclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' 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 -1 '
_cod_original_formula_sum        'C90 H98 Cl4 Fe1 N8 O12'
_cod_database_code               7020579
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
EQUIV PART(1001,OCC) PART(1002,OCC)
WEIGHT -1 PART(1002,OCC)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 12,X'S) H ( 121,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 ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 193,X'S) H ( 192,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 203,X'S) H ( 202,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 ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 292,X'S) H ( 293,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 302,X'S) H ( 303,X'S) H ( 301,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)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 42,X'S) H ( 421,X'S) H ( 422,X'S) H ( 423,X'S)
RIDE C ( 43,X'S) H ( 431,X'S) H ( 432,X'S) H ( 433,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 49,X'S) H ( 491,X'S)
RIDE C ( 50,X'S) H ( 503,X'S) H ( 501,X'S) H ( 502,X'S)
RIDE C ( 51,X'S) H ( 513,X'S) H ( 511,X'S) H ( 512,X'S)
RIDE C ( 52,X'S) H ( 521,X'S)
RIDE C ( 53,X'S) H ( 531,X'S)
RIDE C ( 54,X'S) H ( 541,X'S)
RIDE C ( 55,X'S) H ( 551,X'S)
RIDE C ( 570,X'S) H (5701,X'S) H (5702,X'S)
RIDE C ( 571,X'S) H (5711,X'S) H (5712,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
SAME CL(560) C(570) CL(580) AND
CONT CL(580) C(570) CL(560) AND
CONT CL(561) C(571) CL(581) AND
CONT CL(581) C(571) CL(561)
SIMU 0.01 CL(560) C(570) CL(580) AND
CONT CL(580) C(570) CL(560) AND
CONT CL(561) C(571) CL(581) AND
CONT CL(581) C(571) CL(561)
DELU 0.01 CL(560) C(570) CL(580) AND
CONT CL(580) C(570) CL(560) AND
CONT CL(561) C(571) CL(581) AND
CONT CL(581) C(571) CL(561)
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;