Pre-inverse-crowns: synthetic, structural and reactivity studies of alkali metal magnesiates primed for inverse crown formation
Martínez-Martínez, A. J.; Armstrong, D. R.; Conway, B.; Fleming, B. J.; Klett, J.; Kennedy, A. R.; Mulvey, R. E.; Robertson, S. D.; O'Hara, C. T.; Chemical Science 5 (2014) 771–; doi:10.1039/c3sc52816b

data_1513616
_publ_section_title
;
 Pre-inverse-crowns: synthetic, structural and reactivity studies of
 alkali metal magnesiates primed for inverse crown formation
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              771
_journal_paper_doi               10.1039/c3sc52816b
_journal_volume                  5
_journal_year                    2014
_chemical_formula_sum            'C88 H180 K4 Mg4 N8'
_chemical_formula_weight         1604.04
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                90.00
_cell_angle_beta                 94.132(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.779(3)
_cell_length_b                   25.754(3)
_cell_length_c                   16.135(2)
_cell_measurement_reflns_used    5092
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      74.0466
_cell_measurement_theta_min      3.4294
_cell_volume                     10684(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford Diffraction Gemini S'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37909
_diffrn_reflns_theta_full        70.00
_diffrn_reflns_theta_max         70.00
_diffrn_reflns_theta_min         8.93
_exptl_absorpt_coefficient_mu    2.001
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.997
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3552
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.270
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.718
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         10065
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.717
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.1495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3941
_refine_ls_wR_factor_ref         0.4047
_reflns_number_gt                8302
_reflns_number_total             10065
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3sc52816b.txt
_cod_data_source_block           origsrbf1201
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               1513616