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_7700002
_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_sum            'C252 H318 Mg6 N12 O54 P6'
_chemical_formula_weight         4710.85
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-04-29 deposited with the CCDC.    2019-05-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
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_cell_length_b                   35.8954(11)
_cell_length_c                   17.7162(5)
_cell_measurement_reflns_used    23777
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.3330
_cell_measurement_theta_min      2.8570
_cell_volume                     19768.7(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      120(2)
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_diffrn_measured_fraction_theta_max 0.845
_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  0.0443
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39891
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.183
_diffrn_reflns_theta_min         2.862
_diffrn_source                   'fine-focus sealed X-ray tube'
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_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.738
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             7524
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.418
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         10049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+22.9782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7666
_reflns_number_total             10049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00687g2.cif
_cod_data_source_block           aj0008
_cod_original_cell_volume        19768.7(13)
_cod_database_code               7700002
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              27675