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_7020584
_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         'C39 H39 N5 O5, 2(C H4 O)'
_chemical_formula_sum            'C41 H47 N5 O7'
_chemical_formula_weight         721.85
_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     direct
_audit_creation_date             12-09-13
_audit_creation_method           CRYSTALS_ver_14.40
_cell_angle_alpha                90
_cell_angle_beta                 90.6030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1426(2)
_cell_length_b                   22.5440(4)
_cell_length_c                   11.9542(2)
_cell_measurement_reflns_used    8642
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     3811.16(11)
_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 0.992
_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  0.038
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8649
_diffrn_reflns_theta_full        26.922
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_min         5.106
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.49
_refine_diff_density_min         -0.46
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9587
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8648
_refine_ls_number_restraints     693
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.0004006
_refine_ls_shift/su_mean         0.0000377
_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:
20.8 31.6 15.7 4.07
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1651
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1651
_reflns_limit_h_max              18
_reflns_limit_h_min              0
_reflns_limit_k_max              0
_reflns_limit_k_min              -29
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                5814
_reflns_number_total             8649
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.84
_oxford_diffrn_Wilson_scale      10.76
_oxford_refine_ls_r_factor_ref   0.0932
_oxford_refine_ls_scale          0.3053(3)
_oxford_reflns_number_all        8648
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '2161757 014mwj09'
_cod_data_source_file            c2dt31859h.txt
_cod_data_source_block           27
_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 
;
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_database_code               7020584
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
REM EQUIV PART(1001,OCC) PART(1002,OCC)
REM WEIGHT -1 PART(1002,OCC)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 7,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 13,X'S) H ( 131,X'S)
RIDE C ( 17,X'S) H ( 173,X'S) H ( 172,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S)
RIDE C ( 20,X'S) H ( 201,X'S)
RIDE C ( 21,X'S) H ( 211,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 26,X'S) H ( 261,X'S)
RIDE C ( 31,X'S) H ( 313,X'S) H ( 312,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 33,X'S) H ( 331,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 39,X'S) H ( 393,X'S) H ( 392,X'S) H ( 391,X'S)
RIDE C ( 40,X'S) H ( 401,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 42,X'S) H ( 421,X'S)
RIDE C ( 43,X'S) H ( 431,X'S)
RIDE N ( 46,X'S) H ( 461,X'S)
RIDE C ( 47,X'S) H ( 471,X'S)
RIDE C ( 48,X'S) H ( 482,X'S) H ( 481,X'S) H ( 483,X'S)
RIDE C ( 49,X'S) H ( 492,X'S) H ( 493,X'S) H ( 491,X'S)
RIDE O ( 50,X'S) H ( 501,X'S)
RIDE C ( 51,X'S) H ( 513,X'S) H ( 512,X'S) H ( 511,X'S)
RIDE O ( 52,X'S) H ( 521,X'S)
RIDE C ( 53,X'S) H ( 533,X'S) H ( 531,X'S) H ( 532,X'S)
CONT H ( 534,X'S) H ( 535,X'S) H ( 536,X'S)
RIDE O ( 54,X'S) H ( 541,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE)
LIMIT 0.01000000 U[ISO]
LIMIT 0.01000000 X
LIMIT 0.01000000 Y
LIMIT 0.01000000 Z
LIMIT 0.01000000 U[11]
LIMIT 0.01000000 U[22]
LIMIT 0.01000000 U[33]
LIMIT 0.01000000 U[12]
LIMIT 0.01000000 U[13]
LIMIT 0.01000000 U[23]
LIMIT 0.01000000 OCC
REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE)
END
;