[M(H2O)2(15-crown-5)](NO3)2: A System Rich in Polymorphic and Modulated Phases†
Hao, Xiang; Siegler, Maxime A.; Parkin, Sean; Brock, Carolyn Pratt; Crystal Growth & Design 5 (2005) 2225–; doi:10.1021/cg050312j

data_4505241
_publ_section_title
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 [M(H2O)2(15-crown-5)](NO3)2:&#x2009; A System Rich in Polymorphic and
 Modulated Phases&#x2020;
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_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2225
_journal_paper_doi               10.1021/cg050312j
_journal_volume                  5
_journal_year                    2005
_chemical_formula_moiety         '(C10 H24 O7 Mn 2+), 2(N O3 1-)'
_chemical_formula_sum            'C10 H24 Mn N2 O13'
_chemical_formula_weight         435.25
_chemical_name_systematic        'diaqua(15-crown-5)manganese(II) nitrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1 (1/2*x+1/2*y,1/2*x-1/2*y,-z)'
_symmetry_space_group_name_H-M   'C -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.78(3)
_cell_angle_beta                 126.43(4)
_cell_angle_gamma                89.98(3)
_cell_formula_units_Z            8
_cell_length_a                   14.544(3)
_cell_length_b                   28.470(6)
_cell_length_c                   10.646(2)
_cell_measurement_reflns_used    4918
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     3547(2)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material
;
SHELX97-2 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0149
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11181
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  0.8540
_exptl_absorpt_correction_T_min  0.7921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         8102
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+2.5276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0731
_reflns_number_gt                7133
_reflns_number_total             8102
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg050312jsi20050701_021824.cif
_cod_data_source_block           k03012c
_cod_original_cell_volume        3546.7(18)
_cod_original_sg_symbol_H-M      C-1
_cod_database_code               4505241