On the existence of low-valent magnesium-calcium complexes.
Mai, Jonathan; Rösch, Bastian; Patel, Neha; Langer, Jens; Harder, Sjoerd; Chemical science 14 (2023) 4724–4734; doi:10.1039/d3sc00909b

data_1568862
_publ_section_title
;
 On the existence of low-valent magnesium-calcium complexes.
;
_journal_issue                   18
_journal_name_full               'Chemical science'
_journal_page_first              4724
_journal_page_last               4734
_journal_paper_doi               10.1039/d3sc00909b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C84 H122 Ca2 N4'
_chemical_formula_sum            'C84 H122 Ca2 N4'
_chemical_formula_weight         1268.01
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-08 deposited with the CCDC.	2023-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0659(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.7787(3)
_cell_length_b                   16.8207(2)
_cell_length_c                   14.94992(17)
_cell_measurement_reflns_used    7026
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      72.6650
_cell_measurement_theta_min      2.9310
_cell_volume                     7488.39(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5806
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00  27.00   0.50    0.50    --  -41.48  38.00  60.00  186
  2  \w    -85.00 -55.00   0.50    0.50    --  -41.48 125.00 -30.00   60
  3  \w   -102.00 -18.00   0.50    0.50    --  -41.48 -38.00-120.00  168
  4  \w    148.00 177.00   0.50    1.40    --  104.33  77.00   0.00   58
  5  \w     48.00 105.00   0.50    1.40    --  104.33-125.00-120.00  114
  6  \w     86.00 172.00   0.50    1.40    --  104.33  30.00  30.00  172
  7  \w     28.00 127.00   0.50    1.40    --  104.33 -30.00-150.00  198
  8  \w     81.00 108.00   0.50    1.40    --  104.33-125.00 150.00   54
  9  \w     32.00 122.00   0.50    1.40    --  104.33 -61.00  60.00  180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0278284000
_diffrn_orient_matrix_UB_12      -0.0045025000
_diffrn_orient_matrix_UB_13      0.0867461000
_diffrn_orient_matrix_UB_21      0.0434452000
_diffrn_orient_matrix_UB_22      0.0116302000
_diffrn_orient_matrix_UB_23      -0.0542449000
_diffrn_orient_matrix_UB_31      -0.0041013000
_diffrn_orient_matrix_UB_32      0.0907790000
_diffrn_orient_matrix_UB_33      0.0114911000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0208
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13885
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.705
_diffrn_reflns_theta_min         2.968
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.652
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.403
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.225
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+5.2666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6693
_reflns_number_total             7238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00909b2.cif
_cod_data_source_block           hasj210304a
_cod_depositor_comments
'Adding full bibliography for 1568860--1568864.cif.'
_cod_original_cell_volume        7488.40(15)
_cod_database_code               1568862
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C84H122Ca2N4
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.556
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C17(H17), C28(H28), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C18(H18A,H18B), C20(H20A,H20B), C29(H29A,
 H29B), C31(H31A,H31B), C34(H34A,H34B), C36(H36A,H36B)
2.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C24(H24), C25(H25), C26(H26)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              44913
_shelx_hkl_checksum              40637
_olex2_date_sample_data_collection 2021-03-04
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.245
_oxdiff_exptl_absorpt_empirical_full_min 0.820