Synthesis, structural and magnetic characterisation of a new Mn‒Gd pivalate: preparation from a pre-formed hexanuclear cluster †
Benelli, Cristiano; Murrie, Mark; Parsons, Simon; Winpenny, Richard E. P.; Journal of the Chemical Society, Dalton Transactions  (1999) 4125–; doi:10.1039/a907977g

data_7702431
_publ_section_title
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 Synthesis, structural and magnetic characterisation of a new Mn--Gd
 pivalate: preparation from a pre-formed hexanuclear
 cluster&#x200A;&#x2020;
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_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4125
_journal_paper_doi               10.1039/a907977g
_journal_year                    1999
_chemical_formula_moiety         '[Gd2Mn2(Htma)2(tma)8O2(MeOH)2]CH2Cl2'
_chemical_formula_sum            'C53 H102 Cl2 Gd2 Mn2 O24'
_chemical_formula_weight         1618.63
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.216(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.761(13)
_cell_length_b                   13.423(7)
_cell_length_c                   24.023(10)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    220
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     6972(6)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      220
_diffrn_measured_fraction_theta_full 0.475
_diffrn_measured_fraction_theta_max 0.475
_diffrn_measurement_method       Omega-theta
_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  0.2357
_diffrn_reflns_av_sigmaI/netI    0.2052
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6206
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        +/-5%
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.378
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.272
_exptl_absorpt_correction_type   Difabs
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.010
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4559
_refine_ls_number_restraints     664
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.152
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                2425
_reflns_number_total             4559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907977g.txt
_cod_data_source_block           gdmm84
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' 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 '_atom_sites_solution_primary' value 'Direct methods' was
changed to 'direct'.

data item '_atom_sites_solution_hydrogens' value 'geometric' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               7702431