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_7702432
_publ_section_title
;
 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         '[Dy2Mn2(tma)8(Htma)2O2MeOH)2]CH2Cl2'
_chemical_formula_sum            'C53 H102 Cl2 Dy2 Mn2 O24'
_chemical_formula_weight         1629.13
_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     'Isostructural with Gd analogue'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.15(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.641(9)
_cell_length_b                   13.418(4)
_cell_length_c                   24.024(8)
_cell_measurement_reflns_used    52
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     6935(4)
_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)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.474
_diffrn_measured_fraction_theta_max 0.474
_diffrn_measurement_method       'Omega-theta with learnt profile (Clegg)'
_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  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -2
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -2
_diffrn_reflns_number            9726
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.633
_exptl_absorpt_correction_T_max  0.289
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_type   Psi-scans
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         6135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+26.4775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0687
_reflns_number_gt                5010
_reflns_number_total             6135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907977g.txt
_cod_data_source_block           dymm88
_cod_depositor_comments
;
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_hydrogens' value 'Geometric' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      I2/a
_cod_database_code               7702432