Modulation of the Nuclearity of Molecular Mg(II)-Phosphates: Solid-State Structural Change Involving Coordinating Solvents
Santra, Biswajit; Narayanan, Suriya; Kalita, Pankaj; Kumar, Vierandra; Mandal, Debdeep; Gupta, Vivek; Zimmer, Michael; Huch, Volker; Chandrasekhar, Vadapalli; Scheschkewitz, David; Schulzke, Carola; Jana, Anukul; Dalton Transactions  (2019) –; doi:10.1039/C9DT00687G

data_7700003
_publ_section_title
;
 Modulation of the Nuclearity of Molecular Mg(II)-Phosphates: Solid-State
 Structural Change Involving Coordinating Solvents
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT00687G
_journal_year                    2019
_chemical_formula_moiety
'C144 H164 Mg4 O32 P4, 4(C3 H7 N O), 2(C H Cl3), 8(H2O)'
_chemical_formula_sum            'C158 H210 Cl6 Mg4 N4 O44 P4'
_chemical_formula_weight         3303.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-29 deposited with the CCDC.    2019-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                87.4830(10)
_cell_angle_beta                 76.5730(10)
_cell_angle_gamma                83.5070(10)
_cell_formula_units_Z            1
_cell_length_a                   10.49570(10)
_cell_length_b                   20.6949(3)
_cell_length_c                   21.1795(3)
_cell_measurement_reflns_used    29539
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      28.8630
_cell_measurement_theta_min      2.9610
_cell_volume                     4445.16(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      148(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            100352
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.114
_diffrn_reflns_theta_min         2.474
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
The SQUEEZE/PLATON procedure yielded total void volume and electron 
count of 405\%A^3^ and 105 e, respectively. This falls slightly short 
of equalling two further molecules chloroform per formula (116 e). 
Alternatively one chloroform (58 e) plus one DMF (40 e) or ten water 
molecules (10 e) might be responsible.
The fraction of solvent was treated as a diffuse contribution 
to the overall scattering without specific atom positions.
;
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1254
_refine_ls_number_reflns         20783
_refine_ls_number_restraints     627
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+1.0031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1115
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16087
_reflns_number_total             20783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00687g2.cif
_cod_data_source_block           aj0477
_cod_database_code               7700003
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              81536