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_7700005
_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         'C81 H86 Mg2 N3 O11 P2, C3 H7 N O'
_chemical_formula_sum            'C168 H188 Mg4 N8 O24 P4'
_chemical_formula_weight         2924.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_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                 120.910(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.9635(10)
_cell_length_b                   18.7967(5)
_cell_length_c                   32.9183(11)
_cell_measurement_reflns_used    45586
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.3040
_cell_measurement_theta_min      2.7790
_cell_volume                     15906.9(12)
_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)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            75276
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.603
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64814
_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    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             6208
_exptl_crystal_size_max          0.810
_exptl_crystal_size_mid          0.426
_exptl_crystal_size_min          0.372
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         16454
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0782P)^2^+26.5658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13474
_reflns_number_total             16454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00687g2.cif
_cod_data_source_block           aj0073
_cod_original_cell_volume        15906.9(11)
_cod_database_code               7700005
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.900
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              66989